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Method for producing methacryloxypropyltrimethoxysilane

A kind of technology of methacryloxypropyltrimethoxysilane and methacryloxypropyltrimethoxysilane, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc. , can solve the problems of the by-product sodium chloride salt not being effectively treated, the product yield is not high, the production cost increases, etc., and achieve the effect of low cost, high product yield and easy operation

Active Publication Date: 2015-11-18
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as people have higher and higher requirements for chemical production, low energy consumption, low pollution, safety and environmental protection are required for chemical production, so there are still some problems to be solved in the synthesis of methacryloxypropyltrimethoxysilane by conventional phase transfer catalyst method : The first is that the product yield is not high, generally only 80%-90%; the second is the washing of slag salt, the method of washing with low-boiling solvents such as methanol is generally used in industry, and solvent loss will occur during filtration and distillation, resulting in production costs The third is that the by-product sodium chloride salt has not been effectively treated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 350.0 g of industrial sodium chloride salt to 1000 ml of water, then add 20.0 g of industrial sodium dihydrogen phosphate and 60.0 g of industrial sodium phosphate, stir until completely dissolved, and obtain a saturated aqueous sodium chloride solution with a pH of 7-8 for use.

[0027] Add 2.04mol (405.3g) of chloropropyltrimethoxysilane and 2mol (216.1g) of sodium methacrylate into a 1L four-necked flask, then add 6.1g of tetrabutylphosphorus bromide and 0.6g of 2,6-di-tert Butyl-4-methylphenol, after the feeding is completed, turn on the stirring, the stirring speed is 150 rpm, the temperature of the kettle is increased to 115°C for 3 hours, and then the temperature is lowered to 45°C and filtered to obtain 428.7 g of methacryloyloxy The crude product of propyltrimethoxysilane filtrate, the filter residue is 198.6 grams of sodium chloride. The obtained filtrate is distilled to obtain 407.2 grams of finished product of methacryloxypropyltrimethoxysilane;

[0028] At ...

Embodiment 2

[0031] Add 2.04mol (405.3g) of chloropropyltrimethoxysilane and 2mol (216.1g) of sodium methacrylate into a 1L four-necked flask, then add 6.1g of tetrabutylphosphonium bromide and 0.6g of triphenylphosphorus or 2 ,6-Di-tert-butylphenol, after the feeding is completed, turn on the stirring, the stirring speed is 140 rpm, the temperature of the kettle is increased to 125°C for 4 hours, and then the temperature is lowered to 48°C and filtered to obtain 421.5 g of methacryloyloxy The crude product of propyltrimethoxysilane filtrate, the filter residue is 204.3 grams of sodium chloride. The obtained filtrate was distilled according to the conventional method to obtain 400.4 g of methacryloxypropyl trimethoxysilane product.

[0032] At room temperature, 150.0 grams of the saturated aqueous solution of sodium chloride with a pH of 7-8 obtained in Example 1 was added to 204.3 grams of residue salt, stirred for 5 minutes, filtered, collected the filtrate, and the residue was washed twice...

Embodiment 3

[0035] Add 350 kilograms of industrial sodium chloride salt to 1000 kilograms of water, then add 20 kilograms of industrial sodium dihydrogen phosphate and 60 kilograms of industrial sodium phosphate, and stir until completely dissolved to obtain a saturated aqueous sodium chloride solution with a pH of 7-8 for use.

[0036] Add 2040mol (405 kg) of chloropropyltrimethoxysilane and 2000mol (216 kg) of sodium methacrylate into a 1000L enamel stirred reactor, and then add 6 kg of tetrabutylphosphorus bromide and 0.6 kg of 2,6-di-tert Butyl-4-methylphenol, turn on the stirring, the stirring speed is 130 rpm, the temperature of the kettle is raised to 120°C for 3.5 hours, and then the temperature is lowered to 49°C and filtered to obtain 418 kg of methacryloxypropyl trimethoxy The crude silane filtrate, the filter residue is 203 kg of sodium chloride salt. The obtained filtrate was distilled according to the conventional method to obtain 397 kg of finished product of methacryloxypropy...

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PUM

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Abstract

The invention relates to a method for producing methacryloxypropyltrimethoxysilane, which belongs to the technical field of industry of fine chemicals. The method comprises the following steps: investing gamma-choropropyltrimethoxysilane and sodium methacrylate in a reactor, adding a catalyst and a polymerization inhibitor, stirring and heating for reacting and filtering a reactant, distilling a filtrate to obtain the product; cleaning the filter residue by using saturated common salt brine with PH value to 7-8, filtering, repeating for 2-3 times, and merging a washing lotion for stationary layering, wherein the filter residue is white common salt crystal and can be used for industrial purpose; wherein a lower layer of the washing lotion is saturated common salt brine for next cycle usage; an upper layer of the washing lotion is the methacryloxypropyltrimethoxysilane crude product, and distilling to obtain the product. According to the invention, yield of methacryloxypropyltrimethoxysilane product is high, energy consumption is low, production cost is low, and more importantly, the by-product can be effectively cycled and used, and no environmental pollution is generated.

Description

Technical field [0001] The invention relates to a production method of methacryloxypropyltrimethoxysilane, belonging to the technical field of fine chemicals. Background technique [0002] Methacryloxypropyl trimethoxysilane is a very versatile silane coupling agent product. It is mainly used in industrial fields such as coatings, rubber, plastics, paint, machinery, electronics, etc., to increase adhesion, cross adhesion, Coupling and other functions, and can increase the product's wear resistance, aging resistance and other application properties. This product has a long history of development and is produced by large companies at home and abroad, such as KH-570 from the Chinese Academy of Sciences, Z-6030 from Dow Corning, MEMO from Digosha, KBM-503 from Shin-Etsu, Japan, and A-174 from Momentive There are many patents and reports on the synthesis of methacryloxypropyl trimethoxysilane at home and abroad, such as EP483480B1, EP43753B1, DE-OS4437667, DE-OS44376660, US5103030, E...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 胡江华秦传俊陈圣云汤艳甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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