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Liquid silicon resin and preparation method and application thereof

A liquid silicon and resin technology, applied in the direction of adhesive additives, polymer adhesive additives, etc., can solve the problems of high risk, volatile transportation, difficulties, etc., to reduce the generation of waste acid, wide economic value, high The effect of market value

Active Publication Date: 2014-12-24
LUZHOU NORTH CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Both dimethyldichlorosilane and methyltrichlorosilane have low boiling points, are easy to volatilize and difficult to transport, and because of their large molecular weight, they are easy to form steam clusters, which will burn or explode when they meet open flames, and produce large vapors when they meet water. Defects such as hydrogen chloride gas are very dangerous
[0004] At present, simethicone is used as a plasticizer in the preparation process of silicone sealants to add more reinforcing fillers and increase the strength of silicone rubber products. However, due to the low chemical activity of simethicone, Does not participate in the reaction in the system, resulting in slow oil leakage in the later use of silicone rubber products, which has a great impact on the strength and appearance of the product

Method used

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  • Liquid silicon resin and preparation method and application thereof

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preparation example Construction

[0026] Such as figure 1 Shown, the preparation method of liquid silicone resin of the present invention, the reactor that adopts has stirring and condensation reflux device, comprises the following steps:

[0027] a. Raw material preparation: Methyltrichlorosilane and dimethyldichlorosilane are mixed at a mass ratio of 63:7-27 to obtain a mixed monomer. And reduce the temperature of the reactor to below 5°C. Cooling can use low-temperature circulation tank to cool the raw materials.

[0028] b. Dropping reaction: Add concentrated hydrochloric acid dropwise to the reaction kettle, and control the temperature of the reaction system not to exceed -10-5°C. After the concentrated hydrochloric acid was added dropwise, the reaction was performed until no bubbles were generated, and the reaction system was separated from oil and water.

[0029] The concentration of concentrated hydrochloric acid is preferably 33 to 37%. The dropping speed of concentrated hydrochloric acid can be p...

Embodiment 1

[0041] The mass ratio of dimethyldichlorosilane to methyltrichlorosilane is 9:1; the hydrolysis temperature is 0°C; it is neutralized with sodium carbonate, the dehydration temperature is 140°C, and the pressure is -0.06MPa.

[0042] Add 500 volumes of mixed monomer raw materials into the reaction kettle, cool down to 0° C., and add 200 volumes of concentrated hydrochloric acid dropwise while stirring. After 2 hours, the dropwise addition was completed, and no bubbles were produced after standing for 0.5 hours, and the layers were separated, and the hydrochloric acid at the bottom of the reaction kettle was released, and the concentration of the separated hydrochloric acid was 35%. Add solid sodium carbonate to the oil layer to neutralize to neutral, filter the filtrate and carry out rotary distillation for 3 hours, control the dehydration temperature to 140°C and pressure -0.06MPa to obtain the product. Viscosity is 86mm 2 / s, the refractive index is 1.39, and the volatile m...

Embodiment 2

[0045] The mass ratio of dimethyldichlorosilane to methyltrichlorosilane is 4:1; the hydrolysis temperature is -5°C; it is neutralized with sodium bicarbonate, the delowering temperature is 130°C, and the pressure is -0.09MPa.

[0046] Add 500 volumes of mixed monomer raw materials into the reactor, cool down to -5°C, and add 200 volumes of concentrated hydrochloric acid dropwise while stirring. After 2 hours, the dropwise addition was completed, and no bubbles were produced after standing for 0.5 hours, and the layers were separated, and the hydrochloric acid at the bottom of the reaction kettle was released, and the concentration of the separated hydrochloric acid was 33%. Add solid sodium bicarbonate to the oil layer to neutralize until neutral, filter the filtrate and carry out rotary distillation for 3 hours, control the dehydration temperature to 130°C and pressure -0.09MPa to obtain the product. Viscosity is 115mm 2 / s, the refractive index is 1.41, and the volatile ma...

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Abstract

The invention belongs to the field of synthesis of organosilicone, and specifically relates to liquid silicon resin and a preparation method and application thereof. The liquid silicon resin is particularly applied to the preparation of silicone sealant as a plasticizer replacing simethicone. The preparation method of the liquid silicon resin is prepared through a reaction kettle which is equipped with an agitating device and a condensing reflowing device. The preparation method comprises the following steps: a, preparing raw materials, namely, mixing methyl trichlorosilane and dimethyldichlorosilance, and controlling the temperature of the reaction kettle to be below 5 DEG C; b, dropwise adding and reacting, namely, dropwise adding concentrated hydrochloric acid to the reaction kettle, controlling the temperature of a reaction system to be -10 to 5 DEG C, reacting until no bubble is produced after dropwise adding concentrated hydrochloric acid, and separating oil and water of the reaction system; c, neutralizing oil layer, namely, adding a solid alkaline substance to the oil layer obtained by separating in step b while agitating in order to neutralize the oil layer to reach the neutrality; d, filtering the oil layer, namely, filtering the neutral oil layer obtained in step c, wherein the filtrate is the primary liquid silicon resin; finally refining at low temperature to obtain the refined liquid silicon resin.

Description

technical field [0001] The invention belongs to the field of organosilicon synthesis, and in particular relates to a liquid silicone resin and a preparation method and application thereof. The liquid silicone resin is especially suitable for preparing silicone sealant. Background technique [0002] The main product of the direct synthesis of organosilicon monomer is dimethyldichlorosilane, and a large number of by-products will be produced at the same time, of which dimethyldichlorosilane and methyltrichlorosilane are the two most important components, accounting for 85% respectively. % to 88% and 10% to 15%. [0003] Both dimethyldichlorosilane and methyltrichlorosilane have low boiling points, are easy to volatilize and difficult to transport, and because of their large molecular weight, they are easy to form steam clusters, which will burn or explode when they meet open flames, and produce large vapors when they meet water. Defects such as hydrogen chloride gas are very ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/04C09J11/08
Inventor 张文博李争鸣王勇武孙晓泉徐志远葛强
Owner LUZHOU NORTH CHEM IND
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