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Silicon-hydrogen bond containing hyperbranched polyorganosiloxane and preparation method thereof

A technology of polysiloxane and silicon-hydrogen bond, which is applied in the field of hyperbranched polymer synthesis, can solve the problems of affecting the comprehensive performance of materials and poor storage stability, and achieve the effect of low production cost, cheap price, and easy separation and purification

Inactive Publication Date: 2009-12-30
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the steric hindrance of the group R is small, then R is likely to continue to polymerize at room temperature, the storage stability is poor, and it is easy to release small molecules of water during use, which affects the overall performance of the material.

Method used

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  • Silicon-hydrogen bond containing hyperbranched polyorganosiloxane and preparation method thereof
  • Silicon-hydrogen bond containing hyperbranched polyorganosiloxane and preparation method thereof
  • Silicon-hydrogen bond containing hyperbranched polyorganosiloxane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The specific steps of the technical solution of this embodiment are as follows:

[0030] Under the condition of nitrogen protection and magnetic stirring, add 0.10mol (about 12.20g) trimethoxysilane and 34.25mL methanol to a 100mL four-neck flask in an ice bath, mix well and add 0.96g deionized water and 0.85g concentration 0.1mol / L hydrochloric acid solution, the pH value of the system was adjusted to 4; after the reaction was carried out for 2 hours, solution A was obtained.

[0031] Add 0.09 mol (about 14.58 g) of hexamethyldisiloxane, 1.62 g of deionized water and an appropriate amount of ethanol into a three-necked flask with magnetic stirring, and adjust the pH value of the system to 3 with hydrochloric acid solution; Solution B was obtained after 3 hours of hydrolysis.

[0032] Slowly pour solution B into solution A, and continue to react at 60°C under nitrogen protection for 6 hours to obtain an emulsion; stop heating, pour the emulsion into a separatory funnel...

Embodiment 2

[0034] Under nitrogen protection and stirring conditions, add 16.40g (about 0.10mol) triethoxysilane and 47.62mL ethanol to a 150mL four-necked flask at room temperature, mix well and add 1.98g deionized water and a certain amount of concentrated hydrochloric acid , the pH value of the adjustment system was about 3, and the solution A was obtained after the reaction was carried out for 3 hours.

[0035] Add 18.30g (about 0.12mol) triethoxychlorosilane, 2.16g deionized water and an appropriate amount of ethanol to a three-necked flask with magnetic stirring, and adjust the pH value of the system to 3.5 with hydrochloric acid solution, and hydrolyze at 70°C Solution B was obtained after 2 hours.

[0036] Slowly pour solution B into solution A, and continue to react at 70°C for 8 hours under nitrogen protection to obtain an emulsion; stop heating, pour the emulsion into a separatory funnel and let it stand for 10 hours, then separate to obtain the lower oil , which is a capped h...

Embodiment 3

[0038] Under nitrogen protection and stirring conditions, add 6.10g (about 0.05mol) trimethoxysilane, 8.20g (about 0.05mol) triethoxysilane, 17.34mL methanol and 17.34mL of ethanol, mix well, add 1.15g of deionized water and 1.02g of 0.1mol / L nitric acid solution, adjust the pH value of the system to about 4, and react for 2 hours to obtain solution A.

[0039] Add 24.30 g (about 0.15 mol) of hexamethyldisiloxane, 2.70 g of deionized water and an appropriate amount of methanol into a three-necked flask with magnetic stirring, and adjust the pH of the solution to 4, and hydrolyze it at 80 ° C for 2 hours to obtain Solution B.

[0040] Slowly pour solution B into solution A, and continue to react at 80°C for 10 hours under the protection of nitrogen to obtain an emulsion; stop heating, pour the emulsion into a separatory funnel and let it stand for 9 hours, then separate to obtain the lower layer of oil , which is a capped hyperbranched polysiloxane containing silicon-hydrogen ...

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Abstract

The invention relates to a silicon-hydrogen bond containing hyperbranched polyorganosiloxane and a preparation method thereof. The preparation method comprises the following steps: in terms of mole, under the conditions of nitrogen gas protection and the temperature of between 0 and 30 DEG C, adding alcohol solvents into 100 portions of hydrogenalkoxysilanes; dripping 100 to 130 portions of deionized water into the solution to obtain solution A; dissolving 90 to 150 portions of end capping agent into the alcohol solvents; slowly dripping 90 to 150 portions of deionized water into the mixture; reacting the mixture at a temperature of between 30 and 80 DEG C for constant temperature reaction to obtain solution B; at a temperature of between 60 and 80 DEG C, dripping the solution B into the solution A for reacting for 6 to 10 hours to obtain white emulsion; standing the white emulsion to be completely layered; and separating the mixture to obtain a lower layer of oily matter which is end-capped silicon-hydrogen bond containing hyperbranched polyorganosiloxane with good storage and stable performances. A monomer raw material used by the invention has wide source and low cost; the synchronization method and process are easy to control; the molecular weight is easy to adjust; and the silicon-hydrogen bond containing hyperbranched polyorganosiloxane is suitable for large-scale production and application.

Description

technical field [0001] The invention relates to a silicon-hydrogen bond-containing hyperbranched polysiloxane and a preparation method thereof, in particular to an end-capped silicon-hydrogen bond-containing hyperbranched polysiloxane and a preparation method thereof, belonging to the field of hyperbranched polymer synthesis. Background technique [0002] The unique hyperbranched molecular structure of hyperbranched polysiloxane (HBPSi) has the characteristics of low melt viscosity, high molecular designability and easy preparation. After functional modification of HBPSi with active end groups, it can It is used in many aspects such as catalyst carrier, viscosity regulator, ceramic precursor and luminescent material. Therefore, its synthesis research has become a research hotspot in the field of polymer science research in recent years. The molecular structure of HBPSi contains three structural units including terminal unit, branch unit and linear unit, and there is no entan...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/06
Inventor 梁国正张北京顾嫒娟袁莉
Owner SUZHOU UNIV
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