Alkoxy silicon resin intermediate and preparation method thereof

A technology of silicon alkoxides and intermediates, applied in the field of resin intermediates and their preparation, can solve the problems of difficult transparent products, difficult reaction control, turbid products, etc., and achieves recyclable by-products, convenient transportation, and by-products. less effect

Active Publication Date: 2013-01-23
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the hydroxyl-containing silicone resin intermediate reacts with the organic resin, the hydroxyl group not only reacts with the hydroxyl group of the organic resin, but also undergoes condensation reaction itself, which makes the reaction difficult to control, and sometimes the product is turbid
For example, the hydroxyl silicone resin intermediate reacts with E-44, and after adding a solvent, a transparent product can be obtained, and occasionally a turbid product; and it is difficult to obtain a transparent product by reacting with E-20
And when preparing hydroxyl-containing organic silicon resin intermediates, organochlorosilanes are mainly used to hydrolyze in the presence of solvents such as toluene and xylene, and then separate acid water, and wash the resin liquid to neutrality. This method will produce a large amount of low-concentration acid water 1. The use of organic solvents, etc. will cause environmental pollution, and the obtained silanols need to be stored in solvents, so there are many defects
However, the technology of preparing alkoxy-containing silicone resin intermediates is not yet mature, and there is no effective method for preparing silicone resin intermediates containing certain alkoxy groups.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 150g of methyltrichlorosilane, 230g of phenyltrichlorosilane, and 20g of methylphenyldichlorosilane into the reactor, stir evenly, then add 115g of methanol dropwise into the reactor at a rate of 10Kg / h, and react at 10°C After 3 hours, the temperature was raised to 40°C, 0.04 g of zinc octylate was added, and the reaction was carried out at 90°C for 5 hours to obtain about 250 g of a crude product. Cool down to 80°C, add 20g of water dropwise at a rate of 30Kg / h, react at 80°C for 2 hours, neutralize with sodium methoxide to pH 7, remove volatiles under reduced pressure, maximum temperature 80°C, pressure -0.095Mpa, Add 2g of activated carbon and filter to obtain about 200g of the product. The appearance of the product is a colorless transparent liquid with a viscosity of 150mm 2 / s, the alkoxy content is 8%.

Embodiment 2

[0026] Add 150g of methyltrichlorosilane, 230g of phenyltrichlorosilane, and 365.2g of dimethyldichlorosilane into the reactor, stir evenly, then add 165g of ethanol dropwise to the reactor at a rate of 120Kg / h, and react at 10°C After 5h, 3.73g of ferric chloride was added and reacted at 200°C for 1 hour to obtain about 450g of crude product. Cool down to 80°C, add 20g of water dropwise at a rate of 5Kg / h, react at 100°C for 2 hours, neutralize with sodium ethoxide to pH 8, remove volatiles under reduced pressure, maximum temperature 80°C, pressure -0.095Mpa, Add 2g of activated carbon and filter to obtain 360g of the product. The appearance of the product is a colorless transparent liquid with a viscosity of 120mm 2 / s, alkoxy content 15% (.

Embodiment 3

[0028] Add 301.31g of diphenyldichlorosilane into the reactor, stir evenly, then drop 165g of ethanol into the reactor at a rate of 50Kg / h, react at 0°C for 3h, raise the temperature to 40°C, add 0.6g of zinc naphthalate, React at 50°C for 8 hours, get 320g of the crude product, cool down to 80°C, add 15g of water dropwise at a rate of 10Kg / h, react at 50°C for 3 hours, neutralize with sodium methoxide to pH 6, and decompress to remove volatilization The highest temperature is 180°C, the pressure is -0.1Mpa, add 2g of activated carbon, and filter to obtain 260g of the product. The appearance of the product is a colorless transparent liquid with a viscosity of 10mm 2 / s, the alkoxy content in the product is 15%.

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Abstract

The invention relates to an alkoxy silicon resin intermediate and a preparation method of the alkoxy silicon resin intermediate. The alkoxy silicon resin intermediate contains 8-15% of alkoxy; and the alkoxy silicon resin intermediate is of 10-500mm<2>/S based on the viscosity. The preparation method of the alkoxy silicon resin intermediate comprises steps as follows: (1) adding alcohol to organosilane for alcoholysis reaction; (2) adding a catalyst to a product generated in the alcoholysis reaction for condensing for 1-8 hours at 50-200 DEG C, so as to obtain a condensation product; (3) adding water to the condensation product for hydrolyzing at 30-100 DEG C; and (4) neutralizing until reaching pH (Potential Of Hydrogen) of 6-8, removing methanol in the product, and discoloring and filtering to obtain the alkoxy silicon resin intermediate. The alkoxy silicon resin intermediate provided by the invention is applicable to modified organic resin with active hydroxyl functional group, and also can be directly mixed with a curing agent; the alkoxy silicon resin intermediate is applied to coal coating, appliance paint and other high-temperature resistant products; and with adoption of the preparation method of the alkoxy silicon resin intermediate, less by-products are produced and the preparation method is economic and environment-friendly.

Description

technical field [0001] The invention relates to a resin intermediate and a preparation method thereof, in particular to an alkoxy-containing silicone resin intermediate and a preparation method thereof. Background technique [0002] The basic structural unit (main chain) of traditional silicone polymers is composed of Si-O chain links, and the side chains are connected to various other organic groups through silicon atoms. Therefore, the structure of silicone products contains both "organic groups" and "inorganic structures". This special composition and molecular structure makes it integrate the characteristics of organic substances and the functions of inorganic substances, and has high and low temperature resistance , weather aging resistance, electrical insulation, ozone resistance, water repellency, flame retardant, non-toxic, non-corrosive and physiologically inert, and many other excellent properties, and some varieties also have oil resistance, solvent resistance, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 张建新谭周琴吴国相涂世俭王雯霞龚蓉
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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