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Method for stabilizing silanol group-containing polysiloxane solution, method for producing stabilized silanol group-containing polysiloxane solution, and stabilized silanol group-containing polysiloxane solution

一种聚硅氧烷溶液、硅烷醇基的技术，应用在分子量的稳定化领域，能够解决保存稳定性不充分等问题，达到保存稳定性提高的效果

Active Publication Date: 2016-06-08
NISSAN CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the storage stability of the silanol group-containing polysiloxane solution is not sufficient for the method of adding additives and the method of changing the solvent such as Patent Document 1 and Patent Document 2, and other stabilization methods can be sought.

Method used

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  • Method for stabilizing silanol group-containing polysiloxane solution, method for producing stabilized silanol group-containing polysiloxane solution, and stabilized silanol group-containing polysiloxane solution
  • Method for stabilizing silanol group-containing polysiloxane solution, method for producing stabilized silanol group-containing polysiloxane solution, and stabilized silanol group-containing polysiloxane solution
  • Method for stabilizing silanol group-containing polysiloxane solution, method for producing stabilized silanol group-containing polysiloxane solution, and stabilized silanol group-containing polysiloxane solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～4 and comparative example 1）

[0046] Add 601.5g (2887mmol) of tetraethoxysilane (TEOS), 273.6g (1333mmol) of methyltriethoxysilane (MTEOS) and 44.1g (PhTMOS) into a 3000mL four-neck flask ( 222mmol) and 1324g of acetone, cooled to 10°C under blade stirring, added dropwise 292.2g of 0.01N hydrochloric acid over 20 minutes at 10-20°C, raised the temperature to 62°C, and stirred for 4 hours. To this solution, 1,766 g of PGMEA (propylene glycol monomethyl ether acetate) was added, while concentrating under reduced pressure at 40 to 60°C to replace PGMEA with acetone, hydrogen chloride, water, ethanol, and methanol to obtain 806.3 g PGMEA solution of silanol-containing polysiloxane. Moreover, hydrochloric acid which is a polycondensation catalyst can also be removed by this substitution. The PGME / PGMEA solution of the silanol group-containing polysiloxane was obtained by diluting the PGMEA solution of the silanol group-containing polysiloxane with 1021.3 g of PGME (propylene glycol monomethyl ether). In addit...

Embodiment 5 and comparative example 2）

[0054] Add 185.1g (888.4mmol) of tetraethoxysilane (TEOS) and 264.9g of acetone to a 1000mL four-neck flask, cool to 10°C under blade stirring, and drop 0.01N hydrochloric acid over 20 minutes at 10-20°C 58.43g, heated up to 62°C, and stirred for 4 hours. To this solution, 353.3 g of PGMEA was added, while concentrating under reduced pressure at 40 to 60° C., thereby replacing PGMEA with acetone, hydrogen chloride, water, and ethanol to obtain 159.4 g of silanol group-containing polysiloxane. PGMEA solution. Moreover, hydrochloric acid which is a polycondensation catalyst can also be removed by this substitution. The PGME / PGMEA solution of the silanol group-containing polysiloxane was obtained by diluting the PGMEA solution of the silanol group-containing polysiloxane with 197.3 g of PGME. In addition, the PGME / PGMEA solution of this silanol group-containing polysiloxane was used as the polymer solution of the comparative example 2.

[0055] Next, the PGME / PGMEA solution of...

Embodiment 6 and comparative example 3）

[0061] Add 129.6g (621.9mmol) of tetraethoxysilane (TEOS), 39.6g (222.1mmol) of methyltriethoxysilane (MTEOS), and 8.64g of phenyltrimethoxysilane (PhTMOS) into a 1000mL four-necked flask (43.5mmol), N-(3-(triethoxysilyl)propyl) benzenesulfonamide 0.32g (0.89mmol) and acetone 267.2g, cooled to 10°C under blade stirring, at 10~20°C 59.23 g of 0.01N hydrochloric acid was added dropwise over 20 minutes, the temperature was raised to 62° C., and the mixture was stirred for 4 hours. 356.2 g of PGMEA was added to this solution, while concentrating under reduced pressure at 40 to 60° C., thereby replacing PGMEA with acetone, hydrogen chloride, water, and ethanol to obtain 160.4 g of silanol group-containing polysiloxane. PGMEA solution. Moreover, hydrochloric acid which is a polycondensation catalyst can also be removed by this substitution. The PGEE / PGMEA solution of the silanol group-containing polysiloxane was obtained by diluting the PGMEA solution of the silanol group-containi...

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Abstract

A silanol group-containing polysiloxane solution containing a silanol group-containing polysiloxane is treated with a cation exchange resin in the presence of an alcohol solvent.

Description

technical field [0001] The present invention relates to a method for stabilizing a silanol group-containing polysiloxane solution, a method for producing a stabilized silanol group-containing polysiloxane solution and a stabilized silanol group-containing polysiloxane solution, in particular It relates to a method for stabilizing the molecular weight of silanol group-containing polysiloxane. Background technique [0002] As a method for producing a silanol group-containing polysiloxane used as a coating agent for an antireflection film or the like, it is known to subject a siloxane compound, preferably a siloxane compound, to a siloxane in the presence of a polycondensation catalyst. Alkoxy siloxane or silane polycondensation method. [0003] However, the silanol group-containing polysiloxane solution produced by this method has poor storage stability even if the polycondensation catalyst is deactivated or removed. For example, the molecular weight of the silanol group-cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/32C08K5/05C08L83/06
CPCC08G77/32C08K5/06C08G77/16C08K5/05C08L25/18C08L83/04C08L83/06C08L101/02
Inventor 高濑显司北浩
Owner NISSAN CHEM CORP
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