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Process for preparing an acryloyloxysilane

一种丙烯酰氧基硅烷、烃基的技术，应用在用于制备丙烯酰氧基硅烷领域，能够解决大量时间等问题

Active Publication Date: 2013-06-12
DOW SILICONES CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, filtering the fine particle size and the large amount of metal halide precipitates requires a lot of time, so filtration is a significant bottleneck in commercial-scale production

Method used

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  • Process for preparing an acryloyloxysilane
  • Process for preparing an acryloyloxysilane

Examples

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example

[0082] The following examples are provided to better illustrate the method of the present invention, but the following examples are not to be construed as limiting the invention, which is defined by the appended claims. All parts and percentages reported in the examples are by weight unless otherwise indicated. The following table describes the abbreviations used in the examples:

[0083] Table 1: List of abbreviations used in the examples .

[0084]

[0085]

example 1

[0087]A 500ml three-necked round bottom flask equipped with a mechanical stirrer and thermometer contained 72.5g of a 21% (w / w) NaOEt solution in ethanol. Acrylic acid (16.6 g; 231 mmol) was added dropwise while maintaining the temperature below 25°C. After the acrylic acid addition, the slurry was stirred at ambient temperature for 1 hr. Then the stabilizers PTZ and BHT (each 0.022g), TBAB (2.98g; 9.24mmol), CPTES (55.6g; 231mmol) and mineral spirits (55.6g) (CAS 68551-17-7; C 10-13 isoalkane) into the flask in sequence. The temperature of the reaction mixture was gradually increased up to 140°C while condensing and collecting the low boiling agent (65.5 g) by distillation. The reaction mixture was heated at 140°C for 3 hrs, providing approximately 9% (w / w) sodium chloride in the reaction mixture. GC analysis showed 95% conversion to g-ATE.

[0088] Stirring was stopped and the sodium chloride salt precipitated rapidly and settled completely to give a clear interface betw...

example 2

[0092] Acrylic acid (15.7 kg) was added to 70 kg of a 21 % (w / w) sodium ethoxide solution in ethanol, 61.2 kg of xylene and 30 g of a premix of PTZ, BHT and EDTA-NA. Then 1.2 kg of TBAB and 53 kg of CPTES were added. After distilling ethanol, the reaction mixture was heated at 120° C. for 5 hours to obtain approximately 9% (w / w) sodium chloride in the reaction mixture.

[0093] Water (88.4 g) was poured into 221.0 g of the suspension reaction mixture, resulting in a combined weight percent of sodium chloride in water of about 18%. After brief stirring, the mixture separated into a hazy organic phase and a cloudy salt suspension. A clear solution-solution interface formed within 3 minutes and 191.6 g of organics were decanted, resulting in an 86% organic recovery rate. GC of the organics showed no apparent compositional difference before and after water washing, indicating no measurable hydrolysis of g-ATE. This example shows that metal halides can be removed from g-ATE by w...

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Abstract

The invention provides a process for preparing an acryloyloxysilane, comprising reacting a metal salt of a carboxylic acid having the formula [CR2 2=CR1COO-]aMa+ (I), with a haloorganoalkoxysilane having the formula XR3Si(OR4)nR5 3_n (II) in the presence of mineral spirits and a phase transfer catalyst at a temperature of from 50 to 160 DEG C to form a mixture comprising an acryloyloxysilane and a metal halide having the formula Ma+X- a (III), wherein R1 is H or C1 -C6 hydrocarbyl, each R2 is independently R1 or [COO-]aMa+, Ma+ is an alkali metal cation or alkaline earth metal cation, a is 1 or 2, X is halo, R3 is C1 -C6 hydrocarbylene, each R4 is independently C1 -C10 Q hydrocarbyl, each R5 is independently R1 and n is an integer from 1 to 3.

Description

[0001] Cross references to related patent applications [0002] none technical field [0003] The present invention relates to a process for the preparation of acryloxysilanes, which comprises reacting a metal salt of an unsaturated carboxylic acid with a haloorganoalkoxysilane in the presence of mineral spirits and a phase transfer catalyst to form a a mixture of a halide and an acryloxysilane, and removing at least a portion of the metal halide from the mixture. [0004] The present invention also relates to a method of purifying acryloxysilanes comprising washing the acryloxysilane, a first metal halide and a non-polar A mixture of solvents to produce an organic phase comprising acryloxysilane and an aqueous phase comprising at least a portion of the first metal halide. Background technique [0005] Unsaturated organoalkoxysilanes containing acryloyloxy groups, such as 3-acryloxypropyltriethoxysilane, have been passed through halogenated organoalkoxysilanes and metal sa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
CPCC07F7/1892C07F7/20C07F7/025
Inventor P·胡普费尔德萧冰·周
Owner DOW SILICONES CORP
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