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Multifunctional alkoxy-terminated polysiloxane polymer and preparation method thereof

A technology of polysiloxane and functional alkane, which is applied in the field of polymers, can solve the problems of less alkoxy-terminated silicone oil, affect the quality of silicone oil, reduce the transparency of silicone oil, etc., and achieve the effect of simple preparation process and improved quality

Active Publication Date: 2021-04-30
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The presence of dimethyl sulfoxide in the system will affect the quality of silicone oil, even if the de-lowering treatment is carried out in the later stage, it cannot be completely removed
In addition, KOH is used as the catalyst in this paper, and acid is needed for neutralization at the end, and the generated inorganic salt will exist in the silicone oil, reducing the transparency of the silicone oil
Although it is mentioned in the article that the hydrolysis and condensation of the silane coupling agent is not complete due to insufficient water, and alkoxy-terminated silicone oil will be obtained, the experiments carried out in the paper are all one-time feeding, and only the demonstration of the amount of water is carried out. KOH is used as the catalyst ( KOH) and dimethyl sulfoxide as a cocatalyst, the hydrolysis and condensation process is mainly carried out under the catalysis of KOH, the reaction is faster, the hydrolysis is more thorough, and the alkoxy-terminated silicone oil obtained is less

Method used

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  • Multifunctional alkoxy-terminated polysiloxane polymer and preparation method thereof
  • Multifunctional alkoxy-terminated polysiloxane polymer and preparation method thereof
  • Multifunctional alkoxy-terminated polysiloxane polymer and preparation method thereof

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preparation example Construction

[0068] A method for preparing a polyfunctional alkoxy-terminated polysiloxane polymer, the preparation method comprising: putting in cyclosiloxane, a silane coupling agent and water, performing hydrolytic condensation and prepolymerization, wherein the The silicon atom of the silane coupling agent is connected with an alkoxy group;

[0069] Water and alcohols are removed, and then a catalyst is added to carry out copolymerization and equilibrium ring-opening polymerization to break the media and remove small molecular substances to obtain the polyfunctional alkoxy-terminated polysiloxane polymer. The schematic diagram of the reaction process is as figure 1 shown.

[0070] In the present invention, no additional catalyst is added during the hydrolysis and condensation process, and a strong base catalyst is added after the prepolymerization, dehydration and dealcoholization, which not only prevents the influence of water and alcohol on the catalyst, but also improves the speed ...

Embodiment approach

[0074] As an embodiment of the present invention, the molar ratio n (silane coupling agent) / n (water) of the silane coupling agent to water is 10 -5 ~10 5 , preferably 0.05-20, more preferably 0.1-10.

[0075] As an embodiment of the present invention, the molar ratio n (silane coupling agent) / n (cyclosiloxane) of the cyclosiloxane to the silane coupling agent is 10 -5 ~10 5 , preferably 0.01-100, more preferably 0.1-10.

[0076] In the present invention, the silane coupling agent and cyclosiloxane are put into the reaction container at one time, and the hydrolysis, condensation, prepolymerization and ring-opening polymerization processes are carried out at the same time, and the water, cyclosiloxane and silane coupling agent are adjusted The molar ratio ensures that the silaneoxy groups are not completely hydrolyzed and condensed, controls the viscosity of the silicone oil, and finally obtains a polysiloxane with functional organic groups in the side chain of the polysilox...

Embodiment 1

[0120] Octamethylcyclotetrasiloxane (200g, 0.674mol), aminopropylmethyldiethoxysilane (10g, 0.0524mol), water (0.94g, 0.0524mol) were added to a 500mL three-necked flask to obtain a mixture A, install a spherical condenser and a mechanical stirrer; gradually heat the mixture A to 100°C under heating in an oil bath, and reflux and stir for 6 hours to carry out hydrolysis condensation and prepolymerization to obtain a mixture B; cool the mixture B to room temperature, pass The method of vacuum distillation removes ethanol and residual water produced by hydrolysis in the system at a temperature of 50 ° C and a pressure of 0.01 MPa to obtain a prepolymer; then add tetramethylammonium hydroxide to the prepolymer. Alkali glue (1g, tetramethylammonium hydroxide content 1wt% in alkali glue), under normal pressure and 110 ℃, carry out copolymerization and equilibrium ring-opening polymerization reaction 5 hours, obtain polymer; Heating up to 140 ℃, insulation 30 minutes, Decompose the ...

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Abstract

The invention provides a method for preparing a polyfunctional alkoxy-terminated polysiloxane polymer. The preparation method comprises: putting in cyclosiloxane, a silane coupling agent and water, performing hydrolysis condensation and prepolymerization, Wherein, the silicon atom of the silane coupling agent is connected with an alkoxy group; water and alcohols are removed, and then a catalyst is added to carry out copolymerization and ring-opening polymerization to break the mediator and remove small molecular substances to obtain the poly Functional alkoxy terminated polysiloxane polymer. The invention provides a "one-pot method", using silane coupling agent and cyclosiloxane as raw materials, through hydrolysis, condensation, pre-polymerization and equilibrium polymerization, etc., to prepare a functional organic group in the side chain Alkoxy-terminated polysiloxanes.

Description

technical field [0001] The invention relates to the technical field of macromolecules, in particular to a polyfunctional alkoxy-terminated polysiloxane polymer and a preparation method thereof. Background technique [0002] Alkoxy-terminated polysiloxane polymer, as the preferred polymer for dealcoholized sealants, has more advantages than α, ω-dihydroxypolydimethylsiloxane (107 glue), as shown in: One-component packaging sealants can be prepared; there is no hydroxyl group, which reduces the structural phenomenon caused by hydroxyl groups when blended with fillers; good storage stability. [0003] At present, alkoxy-terminated polysiloxane polymers generally refer to alkoxy-terminated poly(dimethicone) because the synthetic raw material is terminal hydrogen-containing silicone oil or α, ω-dihydroxypolydimethylsiloxane (107 glue). Methylsiloxane, reactive only at the end groups. At the same time, the route adopted is mainly obtained by the addition of silicon hydrosilicon ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/26C08G77/28C08G77/18C08G77/06C08G77/08
CPCC08G77/06C08G77/08C08G77/18C08G77/26C08G77/28
Inventor 卢杭毛贻静陈丽云徐旋喻琮惠袁振乐李露郭昱见金振御
Owner ZHEJIANG XINAN CHEM INDAL GROUP