- Preparation method of high-heat-resistance diepoxide
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The invention discloses a preparation method of a high-heat-resistance diepoxide. The preparation method comprises the following steps: in the presence of 4-toluenesulfonyl chloride and pyridine, reacting 4, 4'- dihydroxydicyclohexane with a metal halide; then carrying out dehalogenation in an alkaline environment to prepare [1, 1' -bis(cyclohexane)]-3, 3' -diene; or in the presence of thiourea, 4, 4apos;-dihydroxy dicyclohexane is subjected to a reaction with halogenated succinimide; then carrying out dehalogenation in an alkaline environment to prepare [1, 1'-bis(cyclohexane)]-3, 3'-diene; and then reacting the[1, 1'-bis(cyclohexane)]-3, 3'-diene with peroxyacetic acid to produce the diepoxide. An existing method has the technical defects of high energy consumption, poor selectivity and the like, isomers exist when a hydroxyl group is dehydrated in a strongly acidic environment, rectification purification is needed, and the product yield is low, and based on the problems, technical innovation is carried out, the hydroxyl group is halogenated firstly, then double bonds are formed in a strongly alkaline environment, post-treatment steps are simplified, and especially, the existence of an isomer is avoided, and the (3, 4, 3 ', 4'-diepoxy)bicyclohexane can be efficiently and conveniently prepared.
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- Bicyclic oxide preparation method (by machine translation)
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The present invention provides bicyclic oxide preparation method, the invention bicyclic oxide catalysting preparation method comprises, hydrogen peroxide and a buffer in the presence of a diene compound epoxidation to prepare bicyclic oxide step. (by machine translation)
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Paragraph 0097; 0098; 0099; 0100; 0110; 0111
(2018/05/16)
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- PHOTOCURABLE COMPOSITION, CURED PRODUCT AND OPTICAL COMPONENT USING SAME
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Provided is a photocurable composition which less causes resin-induced swelling of molds, allows the molds to endure more satisfactorily, and has excellent economic efficiency. This photocurable composition includes components (A), (B), (C), and (D). The component (A) is present in a content of 10 to 50 weight percent of the totality of photocurable compounds contained in the photocurable composition. The component (A) is a cycloaliphatic epoxy compound represented by Formula (a). The component (B) is an oxetane compound having a solubility parameter of 9.5 (cal/cm3)1/2 or more as determined by the Fedors' method. The component (C) is a glycidyl ether epoxy compound having a molecular weight of 250 or more. The component (D) is a photoinitiator: wherein R1 to R18 are each, identically or differently, selected from hydrogen, halogen, a hydrocarbon group optionally containing oxygen or halogen, and optionally substituted alkoxy; and X is selected from a single bond and a linkage group.
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Paragraph 0140-0141
(2018/05/26)
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- Method for producing cyclic olefin compound
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Provided is a method for producing a cyclic olefin compound that makes it possible to suppress isomerization reactions and other such secondary reactions, and to efficiently obtain a high-purity cyclic olefin compound containing few impurities easily and at a high yield. In the method for producing a cyclic olefin compound of the present invention, a cyclic olefin compound having two or more cyclohexene rings in the molecule is produced by intramolecular dehydration of an alicyclic alcohol having two or more hydroxyl-group-bonded cyclohexane rings in the molecule in the presence of a dehydration catalyst, wherein the method is characterized in that a dehydration reaction is carried out while supplying the dehydration catalyst continuously or intermittently to a mixed solution containing the alicyclic alcohol and an organic solvent under reflux of an organic solvent that is azeotropic with water and separates from water at ordinary temperatures, or, when the dehydration catalyst is configured from multiple components, while supplying at least one of these components continuously or intermittently to a mixed solution containing the alicyclic alcohol and an organic solvent.
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Paragraph 0043
(2016/10/09)
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- PREPARATION OF ALICYCLIC DIEPOXIDES
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Embodiments in accordance with the present invention provide alicyclic diepoxide compounds and methods for forming such compounds. Such methods encompass charging a reaction vessel with an appropriate diene and an appropriate dienophile and causing such to react to form and recover a desired alicyclic diepoxide precursor where such precursor is subsequently epoxidized. Such compounds encompass alicyclic diepoxides having purities of at least 95 percent or at least 98 percent with respect non-isomeric residues and are essentially free of any isomeric alicyclic diepoxide residues.
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Page/Page column 18-20
(2010/04/28)
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- PROCESS FOR PRODUCTION OF CYCLIC OLEFINS
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Disclosed is a method for producing a cyclic olefin compound having two or more cyclohexene rings per molecule via intramolecular dehydration of an alicyclic alcohol having two or more hydroxylated cyclohexane rings per molecule. The method includes the step (i) of heating the alicyclic alcohol at a temperature of 130°C to 230°C and a pressure greater than 20 Torr in an organic solvent in the presence of a dehydration catalyst, to carry out dehydration of the alicyclic alcohol while distilling off by-product water, which dehydration catalyst is liquid or soluble in a liquid reaction mixture under the reaction conditions; and the subsequent step (ii) of heating the resulting reaction mixture at a temperature of 50°C to 220°C and a pressure of 200 Torr or less to recover the cyclic olefin compound as a distillate. According to the method, side reactions such as isomerization are suppressed, and high-purity cyclic olefin compounds with less impurities can be simply and efficiently obtained in high yields.
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Page/Page column 14-15; 17
(2009/01/24)
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- ALICYCLIC DIEPOXY COMPOUND, EPOXY RESIN COMPOSITION, AND CURED PRODUCT
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Disclosed is an alicyclic diepoxy compound which gives a cured article suffering from no deterioration in properties even when used in hot and humid surroundings or used under such conditions as to give a strong acid, which is highly reactive upon curing, and which gives a cured article superior typically in thermal stability. Specifically, the alicyclic diepoxy compound includes a 3,4,3',4'-diepoxybicyclohexyl compound represented by following Formula (1): wherein R1 to R18 each represent a hydrogen atom, a halogen atom, a hydrocarbon group which may have an oxygen atom or a halogen atom, or a substituted or unsubstituted alkoxy group, in which the alicyclic diepoxy compound contains isomers of the 3,4,3',4'-diepoxybicyclohexyl compound in a content of less than 20% based on the total of the 3,4,3',4'-diepoxybicyclohexyl compound and the isomers thereof in terms of peak area ratio as determined by gas chromatography.
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Page/Page column 15-17
(2009/04/23)
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- Semiconductor Phostocatalysis. ZnS-Nanocrystallite-Catalyzed Photooxidation of Organic Compounds
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Freshly prepared ZnS (nano-ZnS) suspensions catalyze photooxidation of organic substrates under band-gap irradiation with water as a good electron acceptor, while H2 evolves concomitantly.The organic substrates with hetero atoms or carbon-carbon double bonds (?-bonds), such as triethylamine (TEA), diethylamine (DEA), methanol, ethanol, cyclopentene, cyclohexene, 2-methylfuran, toluene, and ethylbenzene, undergo effective one-hole oxidation.This leads to efficient carbon-carbon bond forming reactions between cumulatively formed radicals at the α-carbon adjacent to the hetero atom or the ?-bond.The photooxidation in the presence of a larger quantity of water results in successive oxidation of the intermediary α-carbon radicals, giving the two-hole oxidation products, e.g., DEA and acetaldehyde from TEA and formaldehyde from methanol.The formation of the intermediary α-carbon radical has been clarified by ESR analysis using 2-propanol as an organic substrate.Semi-empirical molecular orbital calculations suggest that the nano-ZnS-catalyzed photooxidation should be predictable from energetics in the formation of the α-carbon radicals through one-hole oxidation and deprotonation, and from change in the bond order of αC-H bond of the α-carbon cation radicals.
- Yanagida, Shozo,Kawakami, Hiroshi,Midori, Yoshihide,Kizumoto, Hirotoshi,Pac, Chongjin,Wada, Yuji
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p. 1811 - 1824
(2007/10/03)
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