Preparation method of controllable high-molecular-weight MQ silicon resin

A MQ silicone resin, high molecular weight technology, applied in the field of additives, can solve the problems of easy to produce white precipitation, low molecular weight, easy gelation of the system, etc., and achieve the effects of easy molecular weight control, mature technology and fewer reaction by-products.

Inactive Publication Date: 2019-01-08
ZHONGKAI UNIV OF AGRI & ENG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the one hand, it solves the problems that the current traditional silicone resin synthesis method is easy to produce white precipitate, the system is easy to gel, the product is unstable, the molecular weight is not high and it is difficult to control; on the other hand, it fills the current domestic market with high molecular weight MQ silicone resin Rare or absent defects in the product

Method used

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  • Preparation method of controllable high-molecular-weight MQ silicon resin
  • Preparation method of controllable high-molecular-weight MQ silicon resin
  • Preparation method of controllable high-molecular-weight MQ silicon resin

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preparation example Construction

[0045] A preparation method of controllable high molecular weight MQ silicone resin, comprising the following steps:

[0046] (1) Add component A, solvent 1 and catalyst into the reactor, and mix uniformly to form mixed solution C; dissolve component B in solvent 2, stir and mix evenly to form mixed solution D;

[0047](2) Stir the mixed solution C at a constant temperature at any temperature in the range of 30-80°C, with a rotation speed of 200-3000rpm; slowly add the mixed solution D dropwise, and complete the dropwise addition in 30-60 minutes, and then react at a constant temperature for 2-10 hours after the dropwise addition;

[0048] (3) Add reaction inhibitor, stir for 10-50min, remove solvent by vacuum distillation, and obtain MQ silicone resin with controllable high molecular weight;

[0049] The general formula of the component A is:

[0050]

[0051] where: R 1 for C 1 ~C 4 the alkyl group, R 3 and R 4 is aryl, alkyl or arylalkyl; (a 1 +b 1 ) / c 1 The rat...

Embodiment 1

[0073] Add 27.00 g of Component A (see Table 1), 10.80 g of toluene, and 29,000 ppm of Pt catalyst to a 500 ml three-necked flask equipped with a reflux device, an electric heating mantle, a mechanical stirrer, and a dropping funnel, raise the temperature to 50° C., and stir at 300 rpm. 10min; move the mixed solution equipped with 2.00g of component B (see Table 2) and 0.80g of toluene to the dropping funnel, increase the speed of the mixer to 2000rpm and stir at a constant temperature, and add it dropwise to the mixed solution of component A. The dropwise addition was completed in 30 minutes. After the dropwise addition was completed, the reaction was carried out at a constant temperature for 7 hours; then 0.013 g of ethynylcyclohexanol was added and stirred for 20 minutes. After the reaction, the toluene was distilled off under vacuum at 100°C and 0.9MPa, the product was recovered, and dried at 100°C for 2 hours to obtain the MQ silicone resin product. Carry out GPC test to ...

Embodiment 2

[0079] As shown in Group 1 in Table 4, add Component A (see Table 1) 10.00g, toluene 4.00g, Pt catalyst 12000ppm into a 500ml three-necked flask equipped with a reflux device, electric heating mantle, mechanical stirring and dropping funnel , heated up to 50°C, and stirred at 300rpm for 10min; moved the mixed solution equipped with 2.00g of component B (see Table 2) and 0.80g of toluene to the dropping funnel, increased the speed of the mixer to 2000rpm, stirred at a constant temperature, and dropped Add it to the mixed solution of component A, drop it in 30 minutes, and react at constant temperature for 7 hours after the dropwise addition; then add 0.012 g of ethynylcyclohexanol, and stir for 20 minutes. After the reaction was completed, toluene and small molecules were removed by vacuum distillation at 100°C and 0.9 MPa, the product was recovered, and dried at 100°C for 2 hours to obtain the MQ silicone resin product. Carry out GPC test to the product, measure the Mw of the ...

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Abstract

The invention discloses a preparation method of controllable high-molecular-weight MQ silicon resin. The preparation method comprises the following steps: (1) uniformly mixing a component A, a solventI and a catalyst to form mixed liquid C, dissolving a component B in a solvent II, and uniformly stirring and mixing to form mixed liquid D; (2) stirring the mixed liquid C at any temperature between30 DEG C and 80 DEG C at constant temperature, slowly dropwise adding the mixed liquid D for 30 to 60 min, and carrying out constant temperature reaction for 2 to 10 h at the end of dropwise adding;(3) adding a reaction inhibitor, stirring for 10 to 50 min, and distilling the mixture in vacuum to remove the solvent, thus obtaining the controllable high-molecular-weight MQ silicon resin. Preparation of the high-molecular-weight MQ silicon resin and control of the molecular weight can be realized only by adjusting a mole ratio of an active group of the component A to an active group of the component B. According to the preparation method, a few of side products are produced, and recycling of acid, byproducts and the like is not considered; the preparation method is short in production period and high in efficiency and can completely realize industrialization. The product disclosed by the invention is completely dissolved into a polarity or low-polarity solvent, so no problems of sediments and gel which are produced by the system are considered.

Description

technical field [0001] The invention relates to the technical field of additives such as electronic packaging materials, coatings, adhesives, and silicone rubber, and specifically relates to a method for preparing controllable high-molecular-weight MQ silicone resin. Background technique [0002] MQ silicone resin is composed of monofunctional structural unit (R 3 SiO 1 / 2 ) and tetrafunctional structural unit (R 3 SiO 4 / 2 ) Silicone resins formed by covalent bonding. As a new type of silicone polymer material, MQ silicone resin is widely used in silicone rubber reinforcing agent, LED packaging material reinforcing agent, adhesive thickening agent and silicone pressure sensitive adhesive, etc. Increasing the molecular weight of MQ silicone resin is an important way to obtain MQ silicone resin with better performance and better reinforcing effect; while controlling the size of molecular weight is an important way to change the performance of silicone resin from the structu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/12C08G77/06C08G77/08
CPCC08G77/06C08G77/08C08G77/12C08G77/20C08G77/70
Inventor 葛建芳纪建业葛鑫梁伟杰陈循军庞小燕尹国强胡文斌
Owner ZHONGKAI UNIV OF AGRI & ENG
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