- Synthesis of siloxane-based PAMAM dendrimers and luminescent properties of their lanthanide complexes
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The 0.5-2 generations of siloxane-based PAMAM dendrimers with 1, 3-bis(3-aminopropyl) tetramethyldisiloxane (G0) as core unit were synthesized by two different methods. Their structures were characterized by FTIR, 1H NMR, 13C NMR, LC/MS, TGA, and DSC. Results show that method two is more suitable as its synthetic procedure is simple and it provides higher yield than method one. DSC analysis indicates that the introduction of the siloxane linkage into the interior of the dendrimers has significant effect on the flexibility of the dendrimer structures. Lanthanide complexes of the newly designed siloxane-based PAMAM dendrimers were obtained by complexing with Eu(III) and Tb(III), respectively. The luminescent properties of the complexes in the solution were investigated. Narrow-width red and green emissions were observed from the complexes of G0.5, G1.5, and G2.0, indicating intramolecular energy transfer process takes place between ligands and lanthanide ions.
- Niu, Yuzhong,Lu, Haifeng,Wang, Dengxu,Yue, Yuanzhi,Feng, Shengyu
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- Preparation method of diene containing siloxane
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The invention relates to a preparation method of diene containing siloxane. The method includes the steps of performing a hydrosilylation reaction directly in a stainless steel high pressure reaction kettle as a reactor with toluene as a solvent from tetramethyl disiloxane and allylamine as raw materials in the presence of a catalyst; and performing pressure reduced distillation to produce 1,3-bis(gamma-aminopropyl)-1,1',3,3'-tetramethyldisiloxane. The method can ensure that the hydrosilylation reaction between the allylamine and the silicon-hydrogen compound can be carried out directly in one step in a completely water-free and oxygen-free reaction environment, wherein steps of protection and de-protection on an amino group are unnecessary, thereby greatly simplifying the reaction process. Through a self-made Karstedt platinum-containing catalyst, usage amount of the catalyst is reduced and catalytic efficiency is greatly improved. The catalyst has certain addition selectivity, so that isomers in a product can be reduced, thereby increasing yield and reducing cost. The diene containing siloxane reaches 98-99.5% in purity and 75-85% in yield.
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Paragraph 0020; 0021; 0022; 0023; 0024; 0025; 0026-0029
(2017/08/28)
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- A double-end amino (poly) method for the preparation of
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A double-end amino (poly) silicone preparation method, which is characterized in that: the olefin-based primary amine and aromatic or aliphatic formed in ice of phthalic anhydride in acetic acid solvent, for 0 o C-10 o C reaction 1-3h, reflux 3-6h, water, precipitated N-olefin-imide; the molar ratio of 1 : 2.0-5.0 of siloxane and including hydrogen base N-olefin-imide, the aromatic hydrocarbon or alcohol, ether solvent, the presence of a platinum catalyst, for 30 o C-120 o C reaction 3-10h, cooling to room temperature, filter, pressure reducing evaporate the solvent, get [...] imide silicone; the double-phthalimide siloxane dissolved in organic solvent, under the acid catalysis and D 3 or D 4 for 30 o C-100 o C reaction to obtain [...] imide silicone; the double-phthalimide (poly) silicone using ethanol as the solvent, by adding hydrazine hydrate in 60 o C-80 o C reaction 5-15h, filter, pressure reducing evaporate solvent. The process of the invention is simple, normal pressure reaction, non-corrosive material, with little investment; all yield and purity of the product is very high; the solvent can be recycled, the production cost is low, no environmental pollution; by-product of phthalic hydrazide also can be widely applied.
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Paragraph 0033; 0034; 0036
(2017/02/09)
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- Photobase generators derived from trans-o-coumaric acid for anionic UV curing systems without gas generation
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Anionic UV curing systems of poly(glycerol methacrylate) and/or poly[3-(methacryloyloxy)propyltrimethoxysilane] are obtained using novel photobase generators (PBGs) derived from trans-o-coumaric acid. These PBGs decompose into amines and coumarins by UV i
- Arimitsu, Koji,Takemori, Yuri,Nakajima, Atsushi,Oguri, Ayaka,Furutani, Masahiro,Gunji, Takahiro,Abe, Yoshimoto
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p. 1174 - 1177
(2015/04/14)
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- PROCESS FOR THE SYNTHESIS OF 1,3-BIS(AMINOALKYL)DISILOXANES
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The invention provides a process for the synthesis of bis(aminoalkyl)disiloxanes of the general formula I by reaction of the carbamatosilanes of the general formula Ma or of the carbamatodisiloxanes of the general formula Mb or of mixtures thereof in the presence of water, where R1 is a divalent hydrocarbon radical having 1 to 100 C atoms, it being possible for the carbon chain to be interrupted by non-adjacent oxygens, sulphur atoms, —NR6—(CO)— or —NHCONH- groups and for the hydrogens in the divalent hydrocarbon radical individually to be substituted by F, Cl, NR7R8 or OR9 groups, and R2, R3, R4, R5, R6, R7, R8 and R9 are hydrocarbon radicals having 1 to 100 C atoms.
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Page/Page column 3-4
(2012/01/14)
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- IMPROVED PROCESS FOR PRODUCING BIS-(AMINOALKYL)-POLYSILOXANES
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Bis(aminoalkyl)siloxane dimers or oligomers are prepared by a process utilizing hydrosilation of an olefinic amine with tetraorganodisiloxane or with bis(dialkylhydrogen)siloxane oligomers to generate high purity bis(aminoalkyl)disiloxane or bis(aminoalkyl)siloxane oligomers at high conversion yield, which may then be subsequently equilibrated to higher molecular weight bis(aminoalkyl)polysiloxanes.
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Page/Page column 16
(2008/12/07)
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- Method and intermediates for preparation of bis(aminoalkyl)polydiorganosiloxanes
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Silicon-nitrogen compounds are prepared by the reaction of an olefinic amine such as allylamine with a polydiorganosiloxane such as 1,1,3,3-tetramethyldisiloxane, in the presence of a platinum-containing hydrosilation catalyst, preferably a specifically defined platinum complex of 1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasiloxane. Depending on the reaction conditions, the product may be any of several compounds including bis(aminoalkyl)polydiorganosiloxanes and alkenylaminodisiloxanes which are spontaneously converted to cyclic disiloxazanes. The cyclic disiloxazanes may in turn be converted by hydrolysis to bis(aminoalkyl)octaorganotetrasiloxanes.
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- Silyl carbamates and their use in the preparation of bis (aminoalkyl) disiloxanes
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Silyl carbamates are prepared by reacting carbon dioxide with a silazane composition such as 2-methyl-2-sila-3-aza-5-hexene. The silyl carbamates may be converted to symmetrical bis(aminoalkyl)disiloxanes by hydrosilation followed by hydrolysis.
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