- Improvement of a process for preparing peracetic acid by the reaction of acetic acid with hydrogen peroxide in aqueous solutions, catalyzed by ion-exchange resins
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The effect of Amberlyst 15Dry cation-exchange resin on the reaction of peracetic acid formation from acetic acid and hydrogen peroxide in aqueous solution was studied. The pathways of available oxygen consumption were determined. The noncatalytic synthesis is accompanied by spontaneous decomposition of the peracid formed, which sharply decelerates on introducing Amberlyst 15Dry catalyst into the reaction mixture. Comparison of the kinetic relationships of the processes occurring in batch and flow-through reactors shows that in the latter case the process is characterized by diffusion hindrance. A kinetic model of the process with the parameters ensuring adequate mathematical description of the data obtained was suggested.
- Voronov,Sapunov,Makarov,Kulazhskaya,Kaleeva
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Read Online
- MgO/SnO2/WO3 as catalysts for synthesis of ε-caprolactone over oxidation of cyclohexanone with peracetic acid
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Different Mg/Sn/W mixed oxides prepared by precipitation were used as catalysts in the Baeyer-Villiger oxidation of cyclohexanone with a mixture of 50% hydrogen peroxide and acetic acid as oxidant. The Mg/Sn/W oxide obtained by precipitation from NH3·H2O was found to be the catalyst providing the highest yield of ε-caprolactone and initial catalytic activity among all samples.
- Zhang, Guangxu,Ren, Xiaocong,Zhang, Hongbo,Peng, Yu,Gui, Shaoyong
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Read Online
- Synthesis of chromium(III) complex with 1-hydroxy-2-pyridinone-6-carboxylic acid as insulin-mimetic agent and its spectroscopic and computational studies
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The new complex of chromium(III) and 1-hydroxy-2-pyridinone-6-carboxylic acid was synthesized and its preparation routes were reported. Mass spectrometry and elemental analysis indicated the formation of chromium complex with the metal-to-ligand mole ratio of 1:3. Combination of spectroscopic measurement and spectral computations based on the density functional theory suggested that 1-hydroxy-2-pyridinone-6-carboxylic acid was a bidentate ligand using one oxygen atom at pyridinone carbonyl group and the other at N-oxide group as donor atoms upon chelation with chromium(III), forming the six-coordinate complex with five-membered chelate rings. Due to the enhanced stability of the chelate rings, such the pathway of chelation was theoretically predicted to be more favorable than the case where the carboxylate oxygen atom of ligand participated in the chelation. According to the preliminary tests, the chromium(III) complex with 1-hydroxy-2-pyridinone-6-carboxylic acid was found to be active in lowering plasma glucose levels in vivo.
- Yasarawan, Nuttawisit,Thipyapong, Khajadpai,Sirichai, Somsak,Ruangpornvisuti, Vithaya
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Read Online
- Expanding the scope of gallium-catalyzed olefin epoxidation
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The broader use of Ga(III) complexes in the catalysis of olefin epoxidation was explored with a variety of studies. Two Ga(III) complexes with N-donor ligands were found to catalyze olefin epoxidation by peracetic acid in water. The stability of the catalyst more strongly influences the observed reactivity in water than in acetonitrile. Analysis of olefin epoxidation in buffered aqueous solutions indicates that either acidic or basic conditions are necessary for catalysis. The functional group tolerance was assessed using a variety of organic substrates. Alcohols, ketones, and alkylhalides survive the reaction conditions. Other common terminal oxidants were tested as possible replacements for peracetic acid but were not found to benefit from the presence of a Ga(III)-containing catalyst.
- Bronston, Fraser,Ting, Sharon,Zhang, Qiao,Goldsmith, Christian R.
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- Safety advantages of on-site microprocesses
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Usually large-scale capacities are preferred in process industry because of the economics of scale. However, small capacities bring along several other advantages, which are emphasized especially in on-site production. By producing on-site, the transportation of dangerous chemicals can be avoided. Moreover, smaller on-site production processes also mean a step towards inherently safer technology. Microreactors represent a technology that efficiently utilizes safety advantages resulting from small scale. These safety advantages of microreactors in on-site production are studied in this contribution. Production of peracetic acid is used as a test case. This unstable and explosive chemical is used, e.g. in treatment of municipal wastewater and pulp bleaching. This study is based on comparison of a conventional batch process with the capacity of 170 kg/h and an on-site continuous microprocess producing 10 kg/h peracetic acid. Preliminary design of these processes was carried out. Four different methods were used to analyze the safety of the processes. It was found that the conventional methods for analysis of process safety might not be reliable and adequate for radically novel technology, such as microprocesses. This is understandable because the methods are partly based on experience, which is very limited in the connection of totally novel technology. 2009 American Chemical Society.
- Ebrahimi, Fatemeh,Kolehmainen, Eero,Turunen, Ilkka
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- Efficient production of peracetic acid in aqueous solution with cephalosporin-deacetylating acetyl xylan esterase from Bacillus subtilis
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Peracetic acid (PAA) is widely used in sterilization, bleaching textile industry, environmental engineering, chemical synthesis, and biomimetic chemistry. A previous study reported that acetyl xylan esterase (AXE) of Bacillus subtilis CICC 20034 has high activity toward cephalosporin C and 7-aminocephalosporanic acid. In this study, we found that AXE also exhibited high perhydrolysis activity toward acetate esters and endowed itself with great industrial interest on enzyme-catalyzed preparation of PAA. Recombinant AXE of B. subtilis CICC 20034 could be efficiently produced in a low-cost autoinduction medium with an activity of 6.8 × 103 U/mL. The reaction conditions for the optimal synthesis of PAA were as follows: 0.30 mg/mL AXE crude enzyme, 300 mM glycerol triacetate, and 1 M hydrogen peroxide, pH 8.0, and 20 °C, which produced approximately 150 mM of PAA within 5 min. The AXE was then immobilized on an acrylate amino resin; the activity of the immobilized AXE was 383.7 U/g. In the presence of 1 g/mL of immobilized AXE resin, PAA titer of the initial reaction batch was approximately 142.5 mM, and about 95.5 mM of PAA could be produced after 10 cycles.
- Tao, Weiyi,Xu, Qing,Huang, He,Li, Shuang
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Read Online
- A new method for the preparation of peroxyacetic acid using solid superacid catalysts
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A new method for the preparation of peroxyacetic acid from acetic acid and hydrogen peroxide in the presence of solid superacids as a catalyst under mild conditions has been proposed. The preparation of peroxyacetic acid could be carried out in a batchwise operation as well as in a flow-system operation. Nafion-H was found to be active and very stable catalyst for the preparation of peroxyacetic acid and to be regenerated without the loss of catalytic activity.
- Saha, Madhu Sudan,Nishiki, Yoshinori,Furuta, Tsuneto,Denggerile, Ao,Ohsaka, Takeo
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Read Online
- Peracetic acid aqueous solution and method for producing the same
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A peracetic acid aqueous solution and a manufacturing method thereof are provided to be used in various fields including sterilizing washing agents for various medical devices, sterilizing washing agents for food production processes, disinfectants in papermaking processes, semiconductor etching agents, and the like. The peracetic acid solution of claim 1, wherein the peracetic acid solution has 25 weight percent of peracetic acid. The acetic acid of 0.5 ? 15 weight % acetic acid. Hydrogen peroxide 1 through 30 weight percent hydrogen peroxide. An organic acid comprising 1 and 15 weight % of organic acid. The chelating agent 1 according to 5 weight %. , And the remaining water. The chelating agent is selected from the group consisting of [[ [2,1- ethynyl nitrobis (methylene) tetrakis phosphonic acid, [bis amino] methyl phosphonic acid, 2 -phosphonobutane -1 , 2, 4- tricyclic acid, 2 -hydroxy phosphonoacetic acid and mixtures thereof.
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Paragraph 0042-0058
(2021/05/18)
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- Application of Continuous Flow in Tazobactam Synthesis
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Tazobactam is a β-lactamase inhibitor. In this work, a combination of continuous flow and batch experiments for the synthesis of tazobactam has been developed. The first three steps and the preparation of the peroxyacetic acid are continuously carried out in the microreactors, which improves the procedure safety and efficiency. There is also a final step of the deprotection reaction in the microreactor, which can increase the yield and reduce the formation of impurities. Under optimized process conditions, the total yield of the target product reached 37.09% (30.93% in batch). The continuous flow method not only greatly reduces the reaction time but also significantly improves procedure safety and increases the yield.
- Sun, Tiemin,Wang, Jiasheng,Wu, Chengjun,Xin, Yunting,Zhou, Shuhao
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p. 1648 - 1657
(2021/07/19)
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- Preparation method of 4,5-epoxytetrahydrophthalate glycidyl ester
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The present invention provides a method for preparing 4,5-epoxytetrahydrophthalate glycidyl ester. The present invention by taking acetic anhydride as raw material, adding 62.5% ~ 64.7% of hydrogen peroxide and a certain amount of acidic catalyst oxidation to generate peracetic acid, and then the tetrahydrophthalic acid glycidyl ester and the reaction of peracetic acid to obtain epoxy reaction, and then through a series of post-treatments to give 4,5-epoxytetrahydrophthalic acid glycidyl ester. The preparation method of the present invention is compared with the traditional process, which greatly reduces the concentration of hydrogen peroxide, thereby solving the problem that high concentration of hydrogen peroxide in the traditional process is easy to explode during storage, transportation and use, and also reduces the cost of raw materials. Compared with the prior art, the epoxy value of 4,5-epoxytetrahydrothphthalate glycidyl ester products prepared by the present invention is also higher.
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Paragraph 0037-0052
(2022/01/10)
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- Preparation method of 4AA
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The invention discloses a preparation method of 4AA. The preparation method comprises the following steps: S1, preparing a first intermediate from benzamide and a formaldehyde aqueous solution; S2, preparing a second intermediate from the first intermediate, thionyl chloride, toluene and n-heptane; S3, preparing a third intermediate from the second intermediate, methyl acetoacetate, sodium methoxide, toluene, diluted hydrochloric acid and isopropanol; S4, preparing a fourth intermediate from the third intermediate, reductase, ethyl acetate, saturated sodium bicarbonate and saturated salt water; S5, preparing a fifth intermediate from the fourth intermediate, imidazole, TBSCL and methylbenzene; S6, preparing a sixth intermediate from the fifth intermediate, ethanolamine, methanol and n-heptane; S7, preparing a seventh intermediate by using the sixth intermediate, a Grignard reagent and n-heptane; and S8, preparing 4AA from the seventh intermediate, ruthenium trichloride, potassium acetate, ethyl acetate, acetic acid and a peracetic acid solution.
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Paragraph 0016; 0018; 0019; 0021; 0022; 0024; 0025
(2021/07/28)
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- Efficient Assay for the Detection of Hydrogen Peroxide by Estimating Enzyme Promiscuous Activity in the Perhydrolysis Reaction
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Hydrogen peroxide is an ideal oxidant in view of its availability, atom economy, or green aspects. Furthermore, it is produced by the cell mitochondria and plays a meaningful role in controlling physiological processes, but its unregulated production leads to the destruction of organs. Due to its diverse roles, a fast and selective method for hydrogen peroxide detection is the major limitation to preventing the negative effects caused by its excess. Therefore, we aimed to develop an efficient assay for the detection of H2O2. For this purpose, we combined the enzymatic method for the detection of hydrogen peroxide with the estimation of the promiscuity of various enzymes. We estimated the activity of an enzyme in the reaction of p-nitrophenyl esters with hydrogen peroxide resulting in the formation of peracid. To our knowledge, there is no example of a simple, multi-sensor demonstrating the promiscuous activity of an enzyme and detecting hydrogen peroxide in aqueous media.
- Wilk, Monika,Ostaszewski, Ryszard
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p. 1464 - 1469
(2021/02/01)
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- Method for oxidizing acetic acid
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The present disclosure relates to a method for oxidizing acetic acid. The method comprises the step of contacting acetic acid with a peroxide in the presence of a catalyst to perform an oxidation reaction, the catalyst being a catalytic composite material containing carbon dots and titanium oxide. The catalytic composite material containing carbon dots and titanium oxide is used as the catalyst tocatalyze the oxidation reaction of the acetic acid, the acetic acid can be oxidized under mild conditions, the raw material conversion rate and the target product selectivity are high, meanwhile, theeffective utilization rate of peroxide can be remarkably increased, and the production cost is reduced.
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Paragraph 0074-0099
(2020/08/18)
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- Sustainable oxidative cleavage of catechols for the synthesis of muconic acid and muconolactones including lignin upgrading
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Muconic acid and muconolactones are attracting high interest as platform molecules for the synthesis of a variety of compounds, especially in the domain of materials. Although several technologies have been described for their synthesis, there is still a lack of performance, especially regarding green chemistry principles. In this study, we describe the development of an optimized catechol oxidative cleavage to muconic acid using performic acid in an intriguingly safe fashion. Common iron salts were used as catalysts to a level as low as 0.005 mol%, for a maximum turnover number of 13?200. Maximum muconic acid yield reached 84% after isolation by simple filtration. This procedure optimized on catechol was also efficient over a wide range of substituted catechols, providing access to muconolactones in a domino reaction. Noticeably, biobased catechols produced by a proven technology of lignin depolymerization were cleaved into muconolactones of high functional value. Applying this supplementary cleavage step to catechols obtained by lignin depolymerization was thus an ultimate way to maximize the economical value created from lignin. In contrast to other studies, lignin was not only depolymerized, but also depolymerization products were further transformed to take as much value from biomass as possible.
- Coupé, Florentin,Petitjean, Laurène,Anastas, Paul T.,Caijo, Frédéric,Escande, Vincent,Darcel, Christophe
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supporting information
p. 6204 - 6211
(2020/10/18)
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- METHOD OF TREATING DRINKING WATER FOR POULTRY IN THE COURSE OF RAISING THEREOF
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The invention relates to a method of treating water to be supplied to poultry in the course of raising thereof. This method comprises the step of reacting glacial acetic acid and hydrogen peroxide in the presence of a stabilizer to provide a reaction product, letting the reaction product stand until an effective amount of peracetic acid and hydrogen peroxide as active ingredients is formed in the reaction product to thereby obtain a disinfectant. As a result it is provided a continuous flow of water to be supplied to poultry, then continuously the disinfectant is added to the water flow until the concentration of the disinfectant in the water is in the range from 0.025% to 0.065 % to thereby obtain the flow of treated water, and the flow of treated water is maintained to poultry in the course of raising thereof.
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Page/Page column 11
(2021/01/23)
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- ONLINE CONTINUOUS FLOW PROCESS FOR THE SYNTHESIS OF ORGANIC PEROXIDES USING HYDROGEN PEROXIDE AS RAW MATERIAL
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An online continuous flow production process for directly preparing organic peroxides by using hydrogen peroxide as a raw material. This production process uses hydrogen peroxide, catalyst, and an oxidation substrate as a raw material. Substrate will be turned to designated peroxides sequentially through oxidation and workup. This process is performed in a plug-and-produce integrated continuous flow reactor, and the raw materials are continuously fed to the reactor. So, specified peroxide can be continuously obtained at the outlet of the plug-and-produce integrated continuous flow reactor.
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Paragraph 0295
(2020/06/29)
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- Preparation method of penem antibiotic intermediate 4 - acetoxy azacyclobutanone (by machine translation)
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The invention discloses a preparation method of penem antibiotic intermediate 4 - acetoxy azacyclobutanone (4 - AA), and specifically discloses a preparation method of 4 - acetoxyazacyclobutanone (4 - AA) in an organic solvent under the action of a metal catalyst and an oxidant, and has the characteristics of being economical and efficient, small in environmental pollution and high in yield 4 - 4 - AA. (by machine translation)
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Paragraph 0033-0035; 0040-0042; 0048-0052
(2020/09/30)
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- Preparation of Pantoprazole sodium method and Pantoprazole sodium (by machine translation)
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The invention relates to the preparation of Pantoprazole sodium method and pantoprazole sodium. In particular, the invention relates to a method of preparing pantoprazole sodium, comprising the following steps: 1) to 2 - hydroxymethyl - 3, 4 - dimethoxy pyridine (II) as the starting material, in under the action of chloride, the compound of formula III; 2) will be of the formula III compound in the presence of an inorganic base with 5 - difluoro - 2 - mercapto - 1 H - benzimidazole condensation, the compound of formula IV; 3) will be of the formula IV compound is oxidized by an oxidant generating 5 - difluoro - 2 - [(3, 4 - dimethoxy - 2 - pyridyl) methyl] sulfinyl - 1 H - benzimidazole is pantoprazole; 4) the obtained 5 - difluoro - 2 - [(3, 4 - dimethoxy - 2 - pyridyl) methyl] sulfinyl - 1 H - benzimidazole with sodium hydroxide reaction to produce salt that pantoprazole sodium (I); and optionally a 5) the resulting pantoprazole sodium is refined. The method of the invention said product has high purity, and the related impurities such as oxidation impurity, reducing the impurity, decomposition low impurity content. (by machine translation)
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Paragraph 1888
(2019/02/27)
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- A milk lactone perfume continuous compound into method (by machine translation)
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The invention belongs to the technical field of synthetic perfume, and in particular relates to a milk lactone perfume continuous compound into a method, including the role of the alkali under the condition of the aldol reaction, then by hydrogenation reaction, Baeyer - Villiger oxidation, acid continuous hydrolysis, dehydrating and gets milk lactone perfume; the aldol condensation reactions include: part of the as a footing of a cyclohexanone with a alkali mixing, heating processing, the rest [...] butyraldehyde mixture of cyclohexanone with, side drop edge added stirring, and after dropping to continue stirring, thermal insulation reaction-butyraldehyde content to 1% following the end of the reaction; static divider separating the oil, collected and recycled water; collecting oil layer after washing the processing and then transferred to the distillating still distillation recovery excessive cyclohexanone mechanically, the collection of the condensation product of the pan bottom; the invention by adding cyclohexanone in a different way, improving the yield of the aldol condensation reaction; and, of the present invention under the conditions of reaction temperature, can step from an aldol condensation product. (by machine translation)
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Paragraph 0045; 0051; 0052
(2019/05/08)
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- Composition for disinfection and acaricide, and method for controlling of red mite using the same
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The present invention comprises a disinfective and acaricidal composition comprising peracetic acid and saturated fatty acid as active ingredients, and a control method of Dermanyssus gallinae using the same. According to the present invention, pens and poultry farm are disinfected, and the control of Dermanyssus gallinae can be performed quickly and safely at the same time.(S100) Peracetic acid(S200) Mixture of saturated fatty acid and surfactant(S300) Mixture of peracetic acid, saturated fatty acid and surfactantCOPYRIGHT KIPO 2019
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Paragraph 0061-0063
(2019/10/15)
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- A Novel Small Molecule Supports the Survival of Cultured Dopamine Neurons and May Restore the Dopaminergic Innervation of the Brain in the MPTP Mouse Model of Parkinson's Disease
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We previously showed that monoterpenoid (1R,2R,6S)-3-methyl-6-(prop-1-en-2-yl)cyclohex-3-ene-1,2-diol 1 alleviates motor manifestations of Parkinson's disease in animal models. In the present study, we designed and synthesized monoepoxides of (1R,2R,6S)-3-methyl-6-(prop-1-en-2-yl)cyclohex-3-ene-1,2-diol 1 and evaluated their biological activity in the MPTP mouse model of Parkinson's disease. We also assessed the ability of these compounds to penetrate the blood-brain barrier (BBB). According to these data, we chose epoxide 4, which potently restored the locomotor activity in MPTP-treated mice and efficiently penetrated the BBB, to further explore its potential mechanism of action. Epoxide 4 was found to robustly promote the survival of cultured dopamine neurons, protect dopamine neurons against toxin-induced degeneration, and trigger the mitogen-activated protein kinase (MAPK) signaling cascade in cells of neuronal origin. Meanwhile, neither the survival-promoting effect nor MAPK activation was observed in non-neuronal cells treated with epoxide 4. In the MPTP mouse model of Parkinson's disease, compound 4 increased the density of dopamine neuron fibers in the striatum, which can highlight its potential to stimulate striatal reinnervation and thus halt disease progression. Taken together, these data indicate that epoxide 4 can be a promising compound for further development, not only as a symptomatic but also as a neuroprotective and neurorestorative drug for Parkinson's disease.
- Ardashov, Oleg V.,Pavlova, Alla V.,Mahato, Arun Kumar,Sidorova, Yulia,Morozova, Ekaterina A.,Korchagina, Dina V.,Salnikov, Georgi E.,Genaev, Alexander M.,Patrusheva, Oksana S.,Li-Zhulanov, Nikolay S.,Tolstikova, Tat'Yana G.,Volcho, Konstantin P.,Salakhutdinov, Nariman F.
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p. 4337 - 4349
(2019/11/03)
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- 1-methyl-3-(4-diacetoxyl iodobenzene methyl) imidazole chlorine salt as well as preparation and application thereof
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The invention discloses 1-methyl-3-(4-diacetoxyl iodobenzene methyl) imidazole chlorine salt as well as preparation and application thereof. The structure of the 1-methyl-3-(4-diacetoxyl iodobenzene methyl) imidazole chlorine salt is shown in the specification. The invention provides application of the 1-methyl-3-(4-diacetoxyl iodobenzene methyl) imidazole chlorine salt as a gold leaching agent. The application comprises the following steps: putting a sample with a noble metal into the 1-methyl-3-(4-diacetoxyl iodobenzene methyl) imidazole chlorine salt, and performing sufficient stirring so as to leach the noble metal. The 1-methyl-3-(4-diacetoxyl iodobenzene methyl) imidazole chlorine salt which is disclosed by the invention has good capabilities of oxidation and metal coordination, canbe used as the gold leaching agent, breaks through the defect that a toxic gold leaching agent is used in the conventional metallurgical industry, and has the advantages of being efficient, green andenvironment-friendly and sustainable.
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Paragraph 0046; 0049
(2019/12/25)
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- NON-ALPHA SUBSTITUTED PEROXY ACIDS AND USES THEREOF
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The present disclosure is related to non-alpha-substituted, low molecular weight peracid compositions. The peracids have no or a negligible amount of odor, have good stability, and have antimicrobialproperties. The peracid compositions can be formulated into a wide variety of end use products, including disinfectants, sanitizers, sporicides, fungicides, laundry products, hard surface cleaners, bleaching agents, personal cleansers, and water treatment products.
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Paragraph 0065; 0066; 0069
(2018/11/03)
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- SYSTEMS AND METHODS FOR THE CONTINUOUS ON-SITE PRODUCTION OF PEROXYCARBOXCYLIC ACID SOLUTIONS
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Methods and systems for on-site production of peroxycarboxcylic acid compositions, and in particular, nonequilibrium compositions of peracetic acid (PAA) enable the economical and safe production of PAA on-demand at the point of use. The methods and systems control flow rates and proportions of feedstocks/ reactants, perform the required sequence of reaction steps to produce high yield peroxycarboxcylic acid solutions in a continuous manner, and provide optimal reaction time and reactant mixing for continuous and safe on-site production.
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Paragraph 0073; 0074
(2018/03/06)
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- Hard-and-soft phosphinoxide receptors for f-element binding: structure and photophysical properties of europium(iii) complexes
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New phosphinoyl-containing tetradentate heterocycles preorganised for metal ion binding were designed and prepared in high yields. The X-ray structures of two allied phosphinoyl-bearing 2,2′-bipyridyl and phenanthroline ligands, as well as closely related structures of 2,6-bis(diphenylphosphinoyl)pyridine and 9-(diphenylphosphinoyl)-1,10-phenanthroline-2-one, are reported. Complexes of nitrates of several lanthanides and trifluoroacetate of Eu(iii) with two phosphinoyl-bearing 2,2′-bipyridyl and phenanthroline ligands were isolated and characterised. The first structures of lanthanide complexes with phosphinoyl-bearing 2,2′-bipyridyl and phenanthroline ligands are reported. The nature of the counter-ion is crucial for the coordination environment of the metal ion. The photophysical properties of the complexes differring in both the nature of the ligand and counter-ion were investigated. The photophysical properties of the complexes are strongly ligand- and counter-ion-dependent. Absorbance and luminescence excitation spectra of complexes showed main peaks in the UV range which correspond to the absorption of light by the ligand and these are ligand-dependent. Luminescence spectra of complexes show typical europium emission in the red region with a high quantum yield, which orresponds to the transitions5D0→7FJ (J = 0-6). The value of deviation of the components of5D0 →7F2 and5D0 →7F1 transitions from the inversion centre shows a larger dependence on the counter-ion than on the nature of the ligand. The value of the luminescence quantum yield is larger for europium complexes with 2,2′-bipyridyl-based ligands and NO3 counter-ions than for complexes with phenanthroline-based ligands and NO3 counter-ions. A low dependence of the luminescence lifetime of Eu complexes on the nature of the ligand has been demonstrated: values in the solid state were in the range 1.1-2.0 ms.
- Borisova, Nataliya E.,Kharcheva, Anastasia V.,Patsaeva, Svetlana V.,Korotkov, Leonid A.,Bakaev, Sergey,Reshetova, Marina D.,Lyssenko, Konstantin A.,Belova, Elena V.,Myasoedov, Boris F.
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p. 2238 - 2248
(2017/02/26)
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- POLYMERS FROM MUCONIC ACID ISOMERS AND ITS DERIVATIVES
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This invention relates to a process for preparing succinic acid and succinate ester from a succinic acid salt in fermentation broth. In the first stage of this invention, renewable carbon resources are utilized to produce succinic acid through biological fermentation. The succinic acid salt in the fermentation process is subjected to double displacement reaction with a strong acid leading to release of succinic acid. Succinic acid is recovered by fractional crystallization integrated with simulated moving bed chromatography to produce succinic acid and succinate ester.
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Paragraph 0057; 0058
(2017/12/27)
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- Development of Imino-λ3-iodanes with Improved Reactivity for Metal-Free [2+2+1] Cycloaddition-Type Reactions
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Aiming at the enhancement of electrophilicity of imino-λ3-iodanes, we have developed (tosylimino)pentafluorophenyl-λ3-iodane, which shows superior reactivity compared to the commonly used (tosylimino)phenyl-λ3-iodane in the [2+2+1]-type synthesis of imidazoles. (Figure presented.).
- Baba, Takafumi,Takahashi, Shunsuke,Kambara, Yui,Yoshimura, Akira,Nemykin, Victor N.,Zhdankin, Viktor V.,Saito, Akio
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p. 3860 - 3864
(2017/10/09)
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- A kind of activated carbon supported heteropoly acid used for the synthesis of ε-caprolactone
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The invention discloses a method for synthesizing epsilon-caprolactone by using active carbon immobilized heteropoly acid, and belongs to the field of chemical synthesis. The method comprises the following steps: mixing and stirring treated active carbon with a heteropoly acid aqueous solution, rinsing after stirring, and drying, thereby obtaining a catalyst of the active carbon immobilized heteropoly acid; mixing acetic acid, oxydol, a solvent and a stabilizing agent with the catalyst of the active carbon immobilized heteropoly acid; reacting under a vacuum condition after mixing, and distilling off a product namely peroxyacetic acid obtained after the reaction as a distillate to obtain a peroxyacetic acid solution, wherein the stabilizing agent and an ion liquid catalyst are left at the bottom of a reaction kettle as distillation residues; and dropwise adding cyclohexanone into the prepared peroxyacetic acid solution, then reacting under a vacuum condition, and rectifying under the vacuum condition after reacting to obtain epsilon-caprolactone. The yield of a synthesis link of peroxyacetic acid prepared by the method reaches 90-93%, and the yield of the final product namely epsilon-caprolactone is up to 99.2%.
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Paragraph 0066; 0070
(2017/03/08)
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- PROCESS FOR THE EPOXIDATION OF OLEFINS
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The subject invention is related to a process for the epoxidation of olefin with peroxide, comprising reacting peroxide with olefin in the presence a solvent, wherein the solvent has Hansen Solubility Parameters (HSPs) of δT,solvent and δH,solvent and the epoxide product has Hansen Solubility Parameters (HSPs) of δT,product and δH,product, and wherein: [in-line-formulae]δT,product?6≦δT,solvent≦δT,product+6, and[/in-line-formulae] [in-line-formulae]δH,product?6≦δH,solvent.[/in-line-formulae]
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Paragraph 0056-0058
(2016/04/19)
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- Method for preparing acetic acid solution with low water content and high peracetic acid concentration and consecutive preparation device
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The invention discloses a method for preparing an acetic acid solution with low water content and high peracetic acid concentration and a consecutive preparation device. Peracetic acid and percarbamide serve as raw materials, a peracetic acid and sulfuric acid urea aquo-complex is generated under catalysis of concentrated sulfuric acid, then an acetic acid solution of peracetic acid and the sulfuric acid urea aquo-complex are separated through a decompression short-range distillation mode, and the acetic acid solution of peracetic acid with low water content is obtained. The consecutive preparation device comprises a stirring reaction kettle (1), a mixed acid storage tank (2), a short-range distiller (3), a peracetic acid storage tank (4) and an auxiliary material storage tank (5). The raw materials react in the stirring reaction kettle (1) and then are conveyed into the mixed acid storage tank (2); material liquid in the mixed acid storage tank (2) is discharged into the short-range distiller (3), the light-component low-water-content and high-concentration peracetic acid solution is separated and flows into the peracetic acid storage tank (4), and heavy component side products are fed into the auxiliary material storage tank (5). The acetic acid solution prepared through the method is high in peracetic acid content and low in water content.
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Paragraph 0029; 0030
(2017/01/02)
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- An environment-friendly catalyst used for the synthesis of ε-caprolactone
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The invention discloses a method for synthesizing epsilon-caprolactone by using an environment-friendly catalyst, belonging to the technical field of synthesis. The method comprises the following steps: mixing acetic acid, oxydol, a solvent, a stabilizer and an ionic liquid catalyst, reacting at 70-90 DEG C in a vacuum, distilling off the reaction product peroxyacetic acid and solvent as fractions to obtain a peroxyacetic acid solution, wherein the stabilizer and ionic liquid reside on the bottom of the reaction kettle as residues; dropwisely adding cyclohexanone into the peroxyacetic acid solution, reacting at 50-70 DEG C in a vacuum, and separating the reaction solution in a vacuum to obtain the epsilon-caprolactone. By using the method, the yield of the peroxyacetic acid synthesis link is up to 92-95%, and the maximum yield of the end product epsilon-caprolactone is up to 99.6%.
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Paragraph 0025; 0026
(2017/01/05)
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- A high-concentration high-stability of peracetic acid disinfectant and a method for preparing the same
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The invention discloses a high concentration high stability one-element peracetic acid disinfectant and a preparation method thereof, and the high concentration high stability one-element peracetic acid disinfectant consists of the following raw materials by weight: 71%-73% of acetic acid, 1%-3% of hydroxyethylidene diphosphonic acid, 17%-20% of hydrogen peroxide, 1%-3% of sodium glucoheptonate, and balance of water. The preparation method is as follows: adding the acetic acid and the hydroxy ethylidene diphosphonic acid into a reaction kettle, stirring for 5-15min at normal temperature and under normal pressure, slowly adding the sodium glucoheptonate at the temperature no higher than 30 DEG C, stirring until the solution is clear and transparent, standing for 7-10min, adding the hydrogen peroxide, stirring for 10min at normal temperature and under normal pressure to prepare a final solution, curing for 7-10 days at 27-30 DEG C under airtight condition to obtain the one-element peracetic acid disinfectant. The one-element peracetic acid disinfectant is prepared by using hydroxyethylidene diphosphonic acid and sodium glucoheptonate composite stabilizer, by adjusting the formula, peracetic acid concentration is high, stability is good, shelf life is long, recycling cycle is long, hydrogen peroxide content is low, and the problem of secondary emission pollution caused by recycling use can be avoided.
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Paragraph 0025-0027
(2017/03/08)
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- Method for continuously preparing epsilon-caprolactone by utilizing micro-reaction device
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The invention discloses a method for continuously preparing epsilon-caprolactone by utilizing a micro-reaction device. The method comprises the following steps of respectively pumping acetic anhydride and hydrogen peroxide into a micro-reaction stationary bed device which is filled with a catalyst for reaction, and mixing and injecting a discharged material and cyclohexanone into a micro-channel reactor in the micro-reaction device for reaction. Compared with the prior art, the method disclosed by the invention has the advantages that the technology automation degree is high, low carbon, environment protection, energy conservation and emission reduction are realized, and online continuous production for preparing high-concentration peroxyacetic acid is realized; meanwhile, the polymerization of generated epsilon-caprolactone caused as an acid substance is used as the catalyst is avoided, the utilization rate of the acetic anhydride is increased, the selectivity of caprolactone is increased, the reaction time is greatly shortened, the content of a byproduct is reduced, and the safety during a generation process of peroxyacetic acid is greatly increased; meanwhile, the product quality is increased, the utilization rate of a device is effectively increased, and the energy consumption is obviously reduced.
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Paragraph 0047
(2017/02/09)
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- Method and device for preparing anhydrous peroxyacetic acid solution
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The invention discloses a method and device for preparing an anhydrous peroxyacetic acid solution. The method comprises the following steps: reacting percarbamide and excessive acetic acid under the catalytic action of sulfuric acid to generate a peroxyacetic acid-water-urea mixture; distilling the mixture, absorbing moisture from the vapor by using sulfuric acid to obtain anhydrous peroxyacetic acid acetic acid vapor, and cooling the vapor to obtain an anhydrous peroxyacetic acid acetic acid solution; and reacting sulfuric acid with urea to generate a liquid urea sulfate hydrate which resides in the reaction kettle. The device comprises a reaction kettle (1), a rectifying drying tower (2), a cooling tower (3) and a vacuum device (4), wherein the top of the reaction kettle (1) is communicated with the bottom of the rectifying drying tower; the top of the rectifying drying tower is provided with a concentrated sulfuric acid feed port and a vapor outlet; the vapor outlet is communicated with the cooling tower; and the cooling tower is communicated with the vacuum device. Compared with the acetaldehyde oxidation process for preparing the anhydrous peroxyacetic acid solution, the method disclosed by the invention has the advantages of simple technical process, low equipment investment, high safety, environment friendliness and no pollution, and has important practical application value.
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Paragraph 0025; 0026
(2016/12/01)
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- Rhenium-catalyzed dehydrogenative olefination of C(sp3)-H bonds with hypervalent iodine(III) reagents
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A dehydrogenative olefination of C(sp3)-H bonds is disclosed here, by merging rhenium catalysis with an alanine-derived hypervalent iodine(iii) reagent. Thus, cyclic and acyclic ethers, toluene derivatives, cycloalkanes, and nitriles are all successfully alkenylated in a regio- and stereoselective manner.
- Gu, Haidong,Wang, Congyang
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supporting information
p. 5880 - 5884
(2015/06/08)
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- 4-CH3CONH-TEMPO/Peracetic Acid System for a Shortened Electron-Transfer-Cycle-Controlled Oxidation of Secondary Alcohols
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We have developed a 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) derivative catalyzed oxidation of secondary alcohols with peracetic acid as the oxidant, which was generated from H2O2 and acetic acid catalyzed by strongly acidic resins. The oxidation of alcohols proceeded well through a shortened electron-transfer cycle under metal-free conditions, avoiding the use of any other electron-transfer mediators such as halides. In addition, we demonstrated that the present system exhibited excellent efficiency under mild conditions for the oxidation of aromatic, aliphatic, and allylic secondary alcohols. Shortcut to ketones: The 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)-derivative-catalyzed oxidation of secondary alcohols employing peracetic acid generated from H2O2 and acetic acid with strongly acidic resins proceeds through a shortened electron-transfer cycle without halide additives. The system not only exhibits excellent efficiency at room temperature but also has a wide substrate scope.
- Zhang, Shufang,Miao, Chengxia,Xia, Chungu,Sun, Wei
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p. 1865 - 1870
(2015/06/23)
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- METHOD FOR PRODUCING EQUILIBRIUM PERACETIC ACID AND EQUILIBRIUM PERACETIC ACID OBTAINABLE BY THE METHOD
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The invention relates to a method for producing equilibrium peracetic acid by reacting acetic acid with hydrogen peroxide in an aqueous reaction mixture in the presence of methanesulphonic acid as catalyst, and also to the equilibrium peracetic acid obtainable by the method.
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Paragraph 0030
(2015/11/18)
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- NON-CORROSIVE ACETIC PERACID PREPARATION AND PRODUCTION METHOD THEREOF
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PROBLEM TO BE SOLVED: To provide a non-corrosive acetic peracid preparation which is environmentally friendly, has high sterilization property and disinfection property, and suppresses occurrence of corrosion to metals, especially to iron, and a production method thereof. SOLUTION: After a peroxide stock solution to which a trace quantity of polyacrylic acid is added, is mixed with a stock solution of an acetic peracid preparation having a specific composition, the mixture is diluted by water for obtaining the acetic peracid preparation including peroxide, acetic peracid, acetic acid, and polyacrylic acid. The obtained acetic peracid preparation has high sterilization force and disinfection force, and suppresses corrosion action to an iron material and the like. COPYRIGHT: (C)2016,JPOandINPIT
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Paragraph 0043
(2018/11/22)
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- BIOCIDE AND BLEACH COMPOSITIONS AND RELATED METHODS
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Provided are biocide compositions and bleach compositions comprising organic acyl polyoxychlorine and related methods. The reduction of the acyl polyoxychlorine group releases a reactive intermediate that undergoes a series of cascading reduction steps, resulting in termination products Generally Recognized As Safe.
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Paragraph 0296
(2015/07/22)
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- BETA-SUBSTITUTED BETA-AMINO ACIDS AND ANALOGS AS CHEMOTHERAPEUTIC AGENTS
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β-Substituted β-amino acids, β-substituted β-amino acid derivatives, and β-substituted β-amino acid analogs and (bio)isosteres and their use as chemotherapeutic agents are disclosed. The β-substituted β-amino acid derivatives and β-substituted β-amino acid analogs and (bio)isosteres are selective LAT1/4F2hc substrates and exhibit rapid uptake and retention in tumors expressing the LAT1/4F2hc transporter. Methods of synthesizing the β-substituted β-amino acid derivatives and β-substituted β-amino acid analogs and methods of using the compounds for treating cancer are also disclosed. The β-substituted β-amino acid derivatives and β-substituted β-amino acid analogs exhibit selective uptake in tumor cells expressing the LAT1/4F2hc transporter and accumulate in cancerous cells when administered to a subject in vivo. The β-substituted β-amino acid derivatives and β-substituted β-amino acid analogs and (bio)isosteres exhibit cytotoxicity toward several tumor types.
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Paragraph 0705
(2015/09/22)
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- First total synthesis of a guanidine alkaloid Nitensidine D using immobilized ionic liquid, microwaves and formamidinesulfinic acid
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An efficient first total synthesis of a naturally occurring guanidine alkaloid, Nitensidine D isolated from ethanol extract of Pterogyne nitens has been described. Geraniol has been used as the starting material. N-alkylation of phthalimide has been achieved using immobilized ionic liquid and formamidinesulfinic acid acts as the guanylating reagent. [Figure not available: see fulltext.]
- Shallu,Sharma,Singh, Jasvinder
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p. 1869 - 1874
(2015/02/05)
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- New structural motif for carboxylic acid perhydrolases
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Some serine hydrolases also catalyze a promiscuous reaction - reversible perhydrolysis of carboxylic acids to make peroxycarboxylic acids. Five X-ray crystal structures of these carboxylic acid perhydrolases show a proline in the oxyanion loop. Here, we test whether this proline is essential for high perhydrolysis activity using Pseudomonas fluorescens esterase (PFE). The L29P variant of this esterase catalyzes perhydrolysis 43-fold faster (kcat comparison) than the wild type. Surprisingly, saturation mutagenesis at the 29 position of PFE identified six other amino acid substitutions that increase perhydrolysis of acetic acid at least fourfold over the wild type. The best variant, L29I PFE, catalyzed perhydrolysis 83-times faster (kcat comparison) than wild-type PFE and twice as fast as L29P PFE. Despite the different amino acid in the oxyanion loop, L29I PFE shows a similar selectivity for hydrogen peroxide over water as L29P PFE (β0=170 vs. 160 M-1), and a similar fast formation of acetyl-enzyme (140 vs. 62 U mg-1). X-ray crystal structures of L29I PFE with and without bound acetate show an unusual mixture of two different oxyanion loop conformations. The type II β-turn conformation resembles the wild-type structure and is unlikely to increase perhydrolysis, but the type I β-turn conformation creates a binding site for a second acetate. Modeling suggests that a previously proposed mechanism for L29P PFE can be extended to include L29I PFE, so that an acetate accepts a hydrogen bond to promote faster formation of the acetyl-enzyme. Ulterior motif: An esterase variant (L29I; see figure) uses a new mechanism for perhydrolysis of acetic acid, likely involving a second acetate molecule. X-ray crystal structures of L29I PFE with and without bound acetate show an unusual mixture of two different oxyanion loop conformations that creates a binding site for the second acetate. Copyright
- Yin, Delu,Purpero, Vince M.,Fujii, Ryota,Jing, Qing,Kazlauskas, Romas J.
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supporting information
p. 3037 - 3046
(2013/03/28)
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- ACTIVATION OF PEROXYGEN BLEACH
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A peracid bleaching species is formed in situ in aqueous wash liquor by reaction of a peroxygen bleach precursor, such as perborate or percarbonate, and a bleach activator. The bleach activator is an acetylated ethylene diamine, that comprises at least 25% triacetyl ethylene diamine. The peracid is formed more rapidly even at low temperatures (F2) compared to use of conventional pure tetracetyl ethylene diamine (F1) and better disinfectant properties result.
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Page/Page column 1; 13
(2013/12/03)
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- Revised molecular basis of the promiscuous carboxylic acid perhydrolase activity in serine hydrolases
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Several serine hydrolases catalyze a promiscuous reaction: perhydrolysis of carboxylic acids to form peroxycarboxylic acids. The working hypothesis is that perhydrolases are more selective than esterases for hydrogen peroxide over water. In this study, we tested this hypothesis, and focused on L29P-PFE (Pseudomonas fluorescens esterase), which catalyzes perhydrolysis of acetic acid 43-fold faster than wild-type PFE. This hypothesis predicts that L29P-PFE should be approximately 43-fold more selective for hydrogen peroxide than wild-type PFE, but experiments show that L29P-PFE is less selective. The ratio of hydrolysis to perhydrolysis of methyl acetate at different concentrations of hydrogen peroxide fit a kinetic model for nucleophile selectivity. L29P-PFE (β0=170 M-1) is approximately half as selective for hydrogen peroxide over water than wild-type PFE (β0=330 M -1), which contradicts the working hypothesis. An alternative hypothesis is that carboxylic acid perhydrolases increase perhydrolysis by forming the acyl-enzyme intermediate faster. Consistent with this hypothesis, the rate of acetyl-enzyme formation, measured by 18O-water exchange into acetic acid, was 25-fold faster with L29P-PFE than with wild-type PFE, which is similar to the 43-fold faster perhydrolysis with L29P-PFE. Molecular modeling of the first tetrahedral intermediate (Td1) suggests that a closer carbonyl group found in perhydrolases accepts a hydrogen bond from the leaving group water. This revised understanding can help design more efficient enzymes for perhydrolysis and shows how subtle changes can create new, unnatural functions in enzymes. Copyright
- Yin, Delu,Kazlauskas, Romas J.
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experimental part
p. 8130 - 8139
(2012/08/29)
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- A homogeneous gallium(III) compound selectively catalyzes the epoxidation of alkenes
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We demonstrate that a simple gallium(III) complex, [Ga(phen) 2Cl2]Cl (phen = 1,10-phenanthroline), can serve as a homogeneous catalyst for the epoxidation of alkenes. The olefin epoxidations proceed relatively quickly at mild temperatures and, under optimum conditions, are highly selective for the epoxide product.
- Jiang, Wenchan,Gorden, John D.,Goldsmith, Christian R.
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body text
p. 2725 - 2727
(2012/04/23)
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- Investigations on catalytic oxidation of acetaldehyde into peracetic acid in a trickle bed reactor
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Acetaldehyde in liquid phase was oxidized into peracetic acid (PAA) by O2 in a trickle bed reactor in the presence of various organic ferric salts as catalysts. The reaction conditions including temperature, O 2 pressure and concentration of the catalyst were optimized. The results indicate that the yield of PAA can reach about 84% under optimum conditions. Moreover, the effects of solvent type on the reactivity of acetaldehyde were studied. It was found that the reactivity of acetaldehyde varies significantly in different solvent, and acetone is the best solvent for producing PAA. The results were interpreted based on the mechanism and the kinetic behavior of the reaction. The activity coefficient (γ) of acetaldehyde in reactants solution was calculated according to the UNIFAC model and was correlated with the interactions between acetaldehyde and solvent molecules. It is believed that the interactions are the main factors affecting the reactivity of acetaldehyde.
- Wang, Yi,Liu, Bo,Li, Libo,You, Jun,Song, Yongbin
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experimental part
p. 604 - 610
(2012/08/28)
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- CONTINUOUS ON-LINE ADJUSTABLE DISINFECTANT/SANITIZER/BLEACH GENERATOR
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Methods and systems for on-site, continuous generation of peracid chemistry, namely peroxycarboxylic acids and peroxycarboxylic acid forming compositions, are disclosed. In particular, an adjustable biocide formulator or generator system is designed for on-site generation of peroxycarboxylic acids and peroxycarboxylic acid forming compositions from sugar esters. Methods of using the in situ generated peroxycarboxylic acids and peroxycarboxylic acid forming compositions are also disclosed.
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Page/Page column 22
(2012/07/14)
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- METHODS AND COMPOSITIONS FOR THE GENERATION OF PERACETIC ACID ON SITE AT THE POINT-OF-USE
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Methods and compositions for the generation of a peroxyacetic acid sanitizer in proximity to the point-of-use are disclosed. These methods comprise introducing a hydrogen peroxide-acetyl precursor solution to water, mixing, and then adding an aqueous source of a alkali metal or earth alkali metal hydroxide. Triacetin is a preferred acetyl precursor and is converted rapidly and with a high conversion rate into peracetic acid. These methods produce solutions with a high level of peracetic acid. Methods for preparing the hydrogen peroxide- acetyl precursor solution are also provided. Also disclosed are solid compositions comprising a liquid acetyl precursor, a water-soluble source of hydrogen peroxide, and a water-soluble source of alkalinity. The solid composition is a freely-flowable solid that is used as a bleaching agent and a stain remover for the treatment of articles such as fabrics, dentures, textile garments, and equipment used in the food and beverage industry.
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Page/Page column 17
(2012/10/08)
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- Production of peroxycarboxylic acids
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Provided are various methods, systems and reactors for producing peroxycarboxylic acid compositions, such as non-equilibrium compositions of peracetic acid, for example. The methods and systems relate to electrolytic generation of hydrogen peroxide or peroxide ions in a reactor, wherein the generated materials are reacted with an acetyl donor to form peracetic acid. In an embodiment, a source of alkali metal ions is provided to an anode chamber such that the ratio of concentrations of the alkali metal ions to protons in the anode chamber of a reactor is greater than 1.
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Page/Page column 23
(2012/12/13)
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- Branching ratios for the reaction of selected carbonyl-containing peroxy radicals with hydroperoxy radicals
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An important chemical sink for organic peroxy radicals (RO2) in the troposphere is reaction with hydroperoxy radicals (HO2). Although this reaction is typically assumed to form hydroperoxides as the major products (R1a), acetyl peroxy radicals and acetonyl peroxy radicals have been shown to undergo other reactions (R1b) and (R1c) with substantial branching ratios: RO2 + HO2 → ROOH + O2 (R1a), RO 2 + HO2 → ROH + O3 (R1b), RO2 + HO2 → RO + OH + O2 (R1c). Theoretical work suggests that reactions (R1b) and (R1c) may be a general feature of acyl peroxy and α-carbonyl peroxy radicals. In this work, branching ratios for R1a-R1c were derived for six carbonyl-containing peroxy radicals: C2H 5C(O)O2, C3H7C(O)O2, CH3C(O)CH2O2, CH3C(O)CH(O 2)CH3, CH2ClCH(O2)C(O)CH 3, and CH2ClC(CH3)(O2)CHO. Branching ratios for reactions of Cl-atoms with butanal, butanone, methacrolein, and methyl vinyl ketone were also measured as a part of this work. Product yields were determined using a combination of long path Fourier transform infrared spectroscopy, high performance liquid chromatography with fluorescence detection, gas chromatography with flame ionization detection, and gas chromatography-mass spectrometry. The following branching ratios were determined: C2H5C(O)O2, YR1a = 0.35 ± 0.1, YR1b = 0.25 ± 0.1, and YR1c = 0.4 ± 0.1; C3H7C(O)O2, YR1a = 0.24 ± 0.15, YR1b = 0.29 ± 0.1, and YR1c = 0.47 ± 0.15; CH3C(O)CH2O2, Y R1a = 0.75 ± 0.13, YR1b = 0, and YR1c = 0.25 ± 0.13; CH3C(O)CH(O2)CH3, Y R1a = 0.42 ± 0.1, YR1b = 0, and YR1c = 0.58 ± 0.1; CH2ClC(CH3)(O2)CHO, Y R1a = 0.2 ± 0.2, YR1b = 0, and YR1c = 0.8 ± 0.2; and CH2ClCH(O2)C(O)CH3, YR1a = 0.2 ± 0.1, YR1b = 0, and YR1c = 0.8 ± 0.2. The results give insights into possible mechanisms for cycling of OH radicals in the atmosphere.
- Hasson, Alam S.,Tyndall, Geoffrey S.,Orlando, John J.,Singh, Sukhdeep,Hernandez, Samuel Q.,Campbell, Sean,Ibarra, Yesenia
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experimental part
p. 6264 - 6281
(2012/08/28)
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- EPR, 1H and 2H NMR, and reactivity studies of the iron-oxygen intermediates in bioinspired catalyst systems
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Complexes [(BPMEN)FeII(CH3CN)2](ClO 4)2 (1, BPMEN = N,N′-dimethyl-N,N′-bis(2- pyridylmethyl)-1,2-diaminoethane) and [(TPA)FeII(CH 3CN)2](ClO4)2 (2, TPA = tris(2-pyridylmethyl)amine) are among the best nonheme iron-based catalysts for bioinspired oxidation of hydrocarbons. Using EPR and 1H and 2H NMR spectroscopy, the iron-oxygen intermediates formed in the catalyst systems 1,2/H2O2; 1,2/H2O 2/CH3COOH; 1,2/CH3CO3H; 1,2/m-CPBA; 1,2/PhIO; 1,2/tBuOOH; and 1,2/tBuOOH/CH3COOH have been studied (m-CPBA is m-chloroperbenzoic acid). The following intermediates have been observed: [(L)FeIII(OOR)(S)]2+, [(L)FeIV=O(S)]2+ (L = BPMEN or TPA, R = H or tBu, S = CH3CN or H2O), and the iron-oxygen species 1c (L = BPMEN) and 2c (L = TPA). It has been shown that 1c and 2c directly react with cyclohexene to yield cyclohexene oxide, whereas [(L)Fe IV=O(S)]2+ react with cyclohexene to yield mainly products of allylic oxidation. [(L)FeIII(OOR)(S)]2+ are inert in this reaction. The analysis of EPR and reactivity data shows that only those catalyst systems which display EPR spectra of 1c and 2c are able to selectively epoxidize cyclohexene, thus bearing strong evidence in favor of the key role of 1c and 2c in selective epoxidation. 1c and 2c were tentatively assigned to the oxoiron(V) intermediates.
- Lyakin, Oleg Y.,Bryliakov, Konstantin P.,Talsi, Evgenii P.
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body text
p. 5526 - 5538
(2011/08/08)
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- MOLD TREATMENT
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Provided herein is a method for treating a surface contaminated by mold, the method comprising the steps of: mixing a perhydrolase, an ester substrate, a source of hydrogen peroxide and water in suitable amounts to produce a mixture comprising at least 1% by weight peracetic acid; and applying the mixture to a surface contaminated by mold.
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Page/Page column 41-44
(2011/08/08)
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