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Preparation method of polysiloxane fluid containing active hydrogen at single end

A polysiloxane and active hydrogen technology, applied in the field of polysiloxane fluid preparation, can solve the problems of many by-products, high content, and difficult separation of by-products, and achieve mild reaction conditions, few by-products, and high content Effect

Active Publication Date: 2018-12-14
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems that the existing equilibrium polymerization method prepares the polysiloxane fluid containing active hydrogen at one end, the reaction is difficult to control, there are many by-products, and the polysiloxane fluid containing active hydrogen at one end is difficult to separate from the by-product, etc., the present invention The preparation method of polysiloxane fluid containing active hydrogen at one end is proposed. The reaction conditions are mild, and the polysiloxane fluid containing active hydrogen at one end is high in content. It can be combined with Pt catalyst under the action of Pt catalyst without further separation. Silicone polymers containing unsaturated bonds undergo end-capping reactions

Method used

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  • Preparation method of polysiloxane fluid containing active hydrogen at single end
  • Preparation method of polysiloxane fluid containing active hydrogen at single end
  • Preparation method of polysiloxane fluid containing active hydrogen at single end

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Preparation of 1,3-dimethyl-1,1,3,3-tetraphenyldisiloxane: in a 500mL three-necked flask with Pt-100 platinum resistance, mechanical stirring and Teflon stirring paddle In, add 120g (0.496mol) methyldiphenylethoxysilane, 145mL concentration is the LiOH aqueous solution of 5wt%; After the material in the bottle rises from room temperature to 100 ℃ with the speed of 1.25 ℃ / min, under this temperature After reacting for 11 hours, collect the ethanol-water mixed solution produced by the hydrolysis reaction; in order to avoid the increase of LiOH concentration after water evaporation, an appropriate amount of deionized water should be added during the reaction. In the later stage of the reaction, measure the instantaneous refractive index of the distillate at any time, when the refractive index (n D 20 ) when the value was close to 1.3330, the reaction was stopped, and the mixture remaining in the three-necked flask was cooled to room temperature to obtain a white solid...

Embodiment 2

[0055] 50g (0.169mol) D 4Put it into a 100mL three-necked flask, add siloxane quality 1wt% concentrated sulfuric acid as a polymerization catalyst, raise the temperature to 80°C, react for 1h, and then cool to room temperature; 10g (0.042mol) of methyl diphenyl Sodium silanolate is added to concentrated sulfuric acid catalyzed D 4 In the ring-opening polymerization product, the temperature was raised to maintain the reaction temperature at 45°C, and the reaction was carried out under stirring for 5 hours. After cooling to room temperature, it was filtered to obtain 44.5 g of methyldiphenylsiloxy-terminated polysiloxane sodium salt solution, with a yield of 74.2%.

[0056] According to the molar ratio of methyldiphenylsiloxy-terminated polysiloxane sodium salt: dimethylchlorosilane = 1: 1.05, at 20°C, weigh 4.1g (0.043mol) dimethylchlorosilane (Me 2 HSiCl) was added into a 100mL three-necked flask, cooled to 10°C, and 44.5g of methyldiphenylsiloxy-terminated polysiloxane sodiu...

Embodiment 3

[0062] 100g (0.337mol) D 4 Put it into a 250mL three-necked flask, add concentrated sulfuric acid with a siloxane quality of 3.0wt% as a polymerization catalyst, heat up to 65°C, react for 4h, and then cool to room temperature; 12.5g (0.0578mol) of methyl Sodium diphenylsilanolate is added to concentrated sulfuric acid catalyzed D 4 In the ring-opening polymerization product, the temperature was raised to maintain the reaction temperature at 50° C., and the reaction was carried out under stirring for 10 h. After cooling to room temperature, it was filtered to obtain 90.5 g of methyldiphenylsiloxy-terminated polysiloxane sodium salt solution with a yield of 80%.

[0063] According to the molar ratio of methyldiphenylsiloxy-terminated polysiloxane sodium salt: dimethylchlorosilane = 1: 1.05, weigh 5.2g (0.055mol) dimethylchlorosilane (Me 2 HSiCl) was added into a 250mL three-necked flask, cooled to 5°C, and under stirring, 90.5g of methyldiphenylsiloxy-terminated polysiloxane s...

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Abstract

The invention relates to the field of organic chemistry and aims to solve the problems that an existing equilibrium polymerization method for preparing a polysiloxane fluid containing active hydrogenat single end is not easy to control in reaction and produces more byproducts, the polysiloxane fluid containing active hydrogen at single end is difficult to separate from byproducts and the like. The invention provides a preparation method of the polysiloxane fluid containing active hydrogen at the single end. The polysiloxane fluid containing active hydrogen at the single end is prepared from raw materials including octamethylcyclotetrasiloxane, methyl diphenyl alkoxy silane and dimethyl chlorosilane through steps of a cation catalyzed octamethylcyclotetrasiloxane ring-opening polymerization reaction, a replacement reaction, a neutralization reaction and the like, the reaction condition is mild, and the prepared polysiloxane fluid containing active hydrogen at the single end has high content and can be subjected to an end capping reaction with an organic silicon polymer containing unsaturated bonds under the action of a PT catalyst without further separation.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing polysiloxane fluid containing active hydrogen at a single end. Background technique [0002] Active hydrogen-containing polysiloxane fluid (referred to as hydrogen-containing silicone oil) usually refers to the chain end or / and part of the side chain or all side chains of the silicone polymer containing active hydrogen atoms that can participate in the crosslinking reaction ( Si-H bonds), these Si-H bonds can be combined with unsaturated double bonds (such as Si-CH=CH 2 ) or triple bonds (such as Si-C≡CH) monomers, oligomers or polymers undergo hydrosilylation reactions under the action of Pt catalysts to form graft, block or network copolymers. Hydrosilylation reaction is an important way to design and synthesize polymers. After introducing organic functional groups or certain specific structures into polymers by hydrosilylation, it can endow silicone fl...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/06C08G77/08
CPCC08G77/06C08G77/08C08G77/12C08G77/80
Inventor 伍川荣瑞瞿志荣董红邵方君蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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