MQ type silicon resin capable of being quickly cross-linked and cured as well as preparation method and application of MQ type silicon resin

A MQ silicone resin, cross-linking and curing technology, applied in the field of polymer chemistry, to achieve the effect of good application prospects and good structural stability

Active Publication Date: 2022-06-03
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problem that the cross-linking and curing of the existing MQ resin requires the use of expensive platinum vinyl complexes as catalysts to form a cross-linking network, the present invention proposes an MQ type silicone resin that can be cross-linked and cured by utilizing moisture in the air; α-cyanopropyloxyethyloxypropyl functionalized MQ type silicone resin does not need to add platinum, organic tin, organic titanate and other existing catalysts for curing silicone materials, and it will disappear after contact with moisture in the air. Curable, adding a small amount of N,N-dimethyl-p-toluidine as an initiator can achieve fast curing within seconds, with excellent storage stability and fast cross-linking curing performance

Method used

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  • MQ type silicon resin capable of being quickly cross-linked and cured as well as preparation method and application of MQ type silicon resin
  • MQ type silicon resin capable of being quickly cross-linked and cured as well as preparation method and application of MQ type silicon resin
  • MQ type silicon resin capable of being quickly cross-linked and cured as well as preparation method and application of MQ type silicon resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] dry and filled with N 2 In the there-necked flask, add [2-(allyloxy)] ethoxytrimethylsilane of 6.97g (0.0384mol), 20mL toluene and 0.1109g Pt content are the Karstedt catalyst of 2wt%, turn on stirring, at 70 Activated at ℃ for 30 min. Dissolve 20.0 g of commercially available hydrogen-containing MQ resin with a hydrogen content of 0.16 wt% and a viscosity of 4310 cP at 25°C (containing Si-H 0.032 mol) in 20 mL of toluene, and then pass the dissolved clear solution through a syringe pump within 2 hours. It was added dropwise to the reaction system at a uniform rate. After the addition of the materials, the reaction was continued at 70° C. for 3 hours, and the solvent and low boilers were removed to obtain 25.69 g of trimethylsiloxyethoxypropyl-terminated MQ resin.

[0080] The obtained trimethylsiloxyethoxypropyl-terminated MQ resin was mixed with 48.06g (1.5mol) methanol and 1.08g (0.018mol) acetic acid, and the hydroxyl group was deprotected to remove the trimethyls...

Embodiment 2

[0082] dry and filled with N 2 In the three-necked flask, add 13.76g (0.075mol) of [2-(allyloxy)]ethoxytrimethylsilane, 20mL of toluene and 0.1733g of Pt content are the Karstedt catalyst of 2wt%, start stirring, at 70 Activated at ℃ for 30 min. Dissolve 20.0 g of commercially available hydrogen-containing MQ resin with a hydrogen content of 0.25 wt% and a viscosity of 2000 cP at 25°C (containing Si-H 0.050 mol) in 20 mL of toluene, and then pass the dissolved clear solution through a syringe pump within 2 hours. It was added dropwise to the reaction system at a uniform rate. After the addition of the materials, the reaction was carried out at 70° C. for 3 hours, and the solvent and low boilers were removed to obtain 25.30 g of trimethylsiloxyethoxypropyl end-capped MQ resin.

[0083] The obtained trimethylsiloxyethoxypropyl terminated MQ resin was mixed with 80.1 g (2.5 mol) methanol and 1.80 g (0.03 mol) acetic acid, and then the hydroxyl group was deprotected to remove th...

Embodiment 3

[0085] dry and filled with N 2 In the three-necked flask, add 18.30g (0.105mol) of [2-(allyloxy)]ethoxytrimethylsilane, 20mL of toluene and 0.6700g of Pt content as the Karstedt catalyst of 2wt%, start stirring, at 70 Activated at ℃ for 30 min. Dissolve 20.0 g of commercially available hydrogen-containing MQ resin with a hydrogen content of 0.35 wt% and a viscosity of 375 cP at 25°C (containing Si-H 0.070 mol) in 20 mL of toluene, and then pass the dissolved clear solution through a syringe pump within 2 hours. It was added dropwise to the reaction system at a uniform rate. After the addition of materials, the reaction was carried out at 70° C. for 3 hours, and the solvent and low boilers were removed to obtain 28.53 g of trimethylsiloxyethoxypropyl-terminated MQ resin.

[0086] The obtained trimethylsiloxyethoxypropyl end-capped MQ resin was mixed with 99.0g (3.1mol) methanol and 2.2g (0.037mol) acetic acid, and the hydroxyl group was deprotected to remove the trimethylsily...

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Abstract

The invention discloses rapidly cross-linked and cured MQ type silicon resin as well as a preparation method and application thereof. In order to overcome the defects that the existing MQ type silicon resin cannot be cross-linked and cured or a noble metal platinum complex needs to be used during cross-linking and curing or organic tin and organic titanate compounds which have great influence on the environment are used as catalysts, the curing temperature is high and the curing time is long, the invention provides a preparation method of the MQ type silicon resin. According to the invention, the alpha-cyano propyl acyloxyethyl oxypropyl terminated MQ silicon resin is designed and can be quickly crosslinked and cured at room temperature and in the air, and when a small amount of N, N-dimethyl p-benzylamine is added as an accelerant, the alpha-cyano propyl acyloxyethyl oxypropyl terminated MQ silicon resin can be quickly crosslinked and cured within 10s. The organosilicon material formed after cross-linking and curing has no obvious crystallization peak, melting peak and glass transition temperature in the range of-120 to 120 DEG C, has good structural stability, and has good application prospects in the fields of rapid shaping, rapid bonding and the like.

Description

technical field [0001] The invention relates to the field of polymer chemistry, in particular to a fast cross-linking and curing MQ type silicone resin and a preparation method and application thereof. Background technique [0002] The organosilicon polymer material is based on the repeating Si-O-Si chain link of the helical structure as the main chain structure and the side groups are connected with different kinds of organic functional groups, which have excellent thermal stability, high gas permeability, weather resistance, chemical resistance, etc. It is widely used in various fields of aerospace, defense industry and national economy. [0003] At present, silicone polymer materials mainly form a cross-linked and cured network structure through three ways, thereby endowing silicone materials with suitable mechanical and mechanical properties and excellent electrical and hydrophobic properties. The first way is to use hydroxyl-terminated polydimethylsiloxane as the base ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/388
CPCC08G77/38C08G77/388Y02P20/55
Inventor 伍川刘清月郭世平董红张一品王二蕾瞿志荣
Owner HANGZHOU NORMAL UNIVERSITY
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