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Organic silicone thickening agent and preparation method thereof

A technology of organosilicon tackifier and propyltrimethoxysilane, applied in adhesives, polymer adhesive additives, adhesive additives, etc., can solve the problems of inability to remove the chloroplatinic acid catalyst and difficult control of the reaction process, etc. Achieve the effect of good quality, less impurities and wide application fields

Inactive Publication Date: 2018-07-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Or use hydrosilylation reaction to prepare silicone tackifier, the reaction process is not easy to control, and the chloroplatinic acid catalyst in the product cannot be removed

Method used

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  • Organic silicone thickening agent and preparation method thereof
  • Organic silicone thickening agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Take 0.2mol of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 0.1mol of vinyltrimethoxysilane and 0.2mol of hydroxyl-terminated silicone oil into a 250ml three-port with mechanical stirring and temperature controller In the flask, a barium hydroxide monohydrate catalyst accounting for 1% by mass fraction of the total reactants was then added to react at 95° C. for 4 hours.

[0025] (2) After the reaction is finished, the product is suction-filtered under reduced pressure to remove the catalyst, then the filtrate is transferred to a round-bottomed distillation flask, and the low-boiling by-product methanol in the system is removed by vacuum distillation at 100°C / -0.096MPa. Thus a colorless and transparent silicone tackifier is obtained. The detected viscosity is 5.0mpa.s and the refractive index is 1.4133.

Embodiment 2

[0027] (1) Take 0.15mol of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 0.15mol of vinyltrimethoxysilane and 0.2mol of hydroxyl-terminated silicone oil into a 250ml three-port with mechanical stirring and temperature controller In the flask, a barium hydroxide monohydrate catalyst accounting for 1% by mass fraction of the total reactants was then added to react at 95° C. for 4 hours.

[0028] (2) After the reaction is finished, the product is filtered under reduced pressure to remove the catalyst, and then the filtrate is transferred to a round-bottomed distillation flask, and the low-boiling by-product methanol in the system is removed at 100°C / -0.096MPa to obtain Colorless and transparent silicone adhesion promoter. The tested viscosity is 5.5mpa.s and the refractive index is 1.4085.

Embodiment 3

[0030] (1) Take 0.2mol of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 0.1mol of vinyltrimethoxysilane and 0.2mol of hydroxyl-terminated silicone oil into a 250ml three-port with mechanical stirring and temperature controller In the flask, a barium hydroxide monohydrate catalyst accounting for 1% by mass fraction of the total reactants was added and reacted at 100° C. for 4 hours.

[0031] (2) After the reaction is finished, the product is filtered under reduced pressure to remove the catalyst, and then the filtrate is transferred to a round-bottomed distillation flask, and the low-boiling by-product methanol in the system is removed at 100°C / -0.096MPa to obtain Colorless and transparent silicone adhesion promoter. The tested viscosity is 6.0mpa.s and the refractive index is 1.4110.

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Abstract

The invention discloses a preparation method for an organic silicone thickening agent. The method comprises the following steps: (1) using dimethyl terminal hydroxy silicone oil, vinyl trimethoxy silane and 3-glycidoxypropyltrimethoxysilane as raw materials, adding barium hydroxide monohydrate, and performing a non-hydrolytic sol-gel reaction under heating and stirring conditions to prepare a crude product of the thickening agent; and (2) firstly performing reduced-pressure filtration on the crude product prepared in the step (1), and performing reduced-pressure distillation on the filtrate, so as to prepare the organic silicone thickening agent. The prepared organic silicone thickening agent provided by the invention is a colorless transparent viscous liquid, has low viscosity and is easyto use; and the preparation process has simple operation and good repeatability and controllability, does not use an organic solvent, saves energy, protects the environment, can obviously improve bonding strength between silicone rubber and a copper substrate, and has good compatibility.

Description

technical field [0001] The invention belongs to the technical field of organosilicon industry, in particular to a method for preparing an organosilicon tackifier. Background technique [0002] The electronic encapsulation glue will assemble and connect the various components of the electronic equipment according to the process requirements to achieve the purpose of isolating the external environment such as water and oxygen, thereby protecting the internal electronic devices. Addition-type vulcanized silicone rubber has been widely used in many fields such as electronic potting glue and liquid injection molding glue because of its excellent high and low temperature resistance, humidity resistance, ozone resistance, weather resistance and electrical insulation properties. However, the molecular chain of polydimethylsiloxane (the chemical component of silicone rubber) presents a helical coil shape, and in the outer layer of the helix, there are many methyl groups around, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C09J11/08C09J183/07C09J183/05
CPCC08G77/44C08L2205/02C08L2205/025C08L2205/03C09J11/08C09J183/04C08L83/04C08L83/10
Inventor 潘朝群孙锐
Owner SOUTH CHINA UNIV OF TECH
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