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Preparation method of acidic cross-linking agent

A cross-linking agent and acidic technology, which is applied in the field of preparation of acidic cross-linking agents, can solve the problems that free chlorine is difficult to control, difficult to handle, difficult to purchase raw materials, etc.

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

[0009] The main advantage of this method is that the reaction is simple and there is no side reaction, but the raw materials are not easy to purchase and are relatively expensive, and the corrosive by-product acetyl chloride that is not easy to handle is produced, and the free chlorine of the product is not easy to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 2000ml three-necked flask connected with a magnetic stirrer, a distillation head, a straight condenser (connected with cooling tap water), a single-strand vacuum tailpiece, and a 1000ml single-mouth receiving flask, add 492g of propyltrimethoxysilane, 540g of glacial acetic acid and 0.03 g hexamethylphosphoric triamide, heat up to 75°C at a stirring speed of 100 rpm, keep the temperature for 6 hours, keep normal pressure throughout the reaction, a small amount of methanol is collected in the receiving bottle during the reaction; after the reaction is completed The crude product obtained by the reaction was subjected to atmospheric distillation at a pressure of 101KPa and a temperature of 75°C. The atmospheric distillation time was 2h, and 256g of methanol, a by-product of the transesterification reaction, was collected. Carry out vacuum distillation again under the conditions, collect residual low boiling 50g, obtain propyl triacetoxysilane crude product; The obtain...

Embodiment 2

[0024] In a 2000ml three-necked flask connected with a magnetic stirrer, a distillation head, a straight condenser (connected with cooling tap water), a single-strand vacuum tailpiece, and a 1000ml single-mouth receiving flask, add 492g of propyltrimethoxysilane, 540g of glacial acetic acid, and 0.03 g hexamethylphosphoric triamide, heat up to 70°C at a stirring speed of 90 rpm, keep the temperature for 5 hours, keep normal pressure throughout the reaction, a small amount of methanol is collected in the receiving bottle during the reaction; after the reaction is completed The crude product obtained by the reaction was subjected to atmospheric distillation at a pressure of 101KPa and a temperature of 120°C. The atmospheric distillation time was 1.5h, and 250g of methanol by-product of the transesterification reaction was collected. Under the condition of ℃, carry out vacuum distillation again, collect residual low boiling 70g, obtain propyl triacetoxysilane crude product; The ob...

Embodiment 3

[0026] In a 2000ml three-necked flask connected with a magnetic stirrer, a distillation head, a straight condenser (connected with cooling tap water), a single-strand vacuum tailpiece, and a 1000ml single-mouth receiving flask, add 492g of propyltrimethoxysilane, 540g of glacial acetic acid, and 0.05 g hexamethylphosphoric triamide, heat up to 60°C at a stirring speed of 100 rpm, keep the temperature for 5 hours, keep normal pressure throughout the reaction, a small amount of methanol is collected in the receiving bottle during the reaction; after the reaction is completed The crude product obtained by the reaction was subjected to atmospheric distillation at a pressure of 101KPa and a temperature of 90°C. The atmospheric distillation time was 1.5h, and 248g of methanol, a by-product of the transesterification reaction, was collected. Under the condition of ℃, carry out vacuum distillation again, collect residual low boiling 63g, obtain propyl triacetoxysilane crude product; Th...

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Abstract

The invention relates to a preparation method of an acidic cross-linking agent, which belongs to the technical field of organic chemistry. According to the invention, propyl trimethoxy silane and glacial acetic acid are taken as raw materials; hexamethylphosphoric triamide is taken as a catalyst, the acidic cross-linking agent product can be synthesized through a group exchange reaction, in the reaction process, by-product methanol is steamed out of the reaction system, and chemical reaction moves to the direction of generation of the acidic cross-linking agent. The method is a substitution method of the acidic cross-linking agent, the method technology is simple and is suitable for industrial scale production, compared with the current preparation method of the acidic cross-linking agent, the by-product with strong corrosivity and difficult treatment can not be generated; no side reaction for influencing the product quality of the acidic cross-linking agent is generated; especially the product content. In addition, the raw materials do not contain chlorine, so that the prepared acidic cross-linking agent product has low free chlorine.

Description

technical field [0001] The invention relates to a preparation method of an acidic crosslinking agent, belonging to the technical field of organic chemistry. Background technique [0002] Acidic crosslinking agent is a kind of silane coupling agent. Its acyloxy group is more active than other groups such as methoxyl and ethoxyl. It has faster decomposition speed and better hydrolysis, which is beneficial to improve operation efficiency. The acetic acid produced by hydrolysis is weaker in acidity and less harmful to the reaction system. Therefore, it has a better bonding effect on strengthening aluminum alloy, nylon, glass and ceramics. It is mainly used as a crosslinking agent for RTV-1 silicone rubber sealant; a surface treatment agent for glass fibers; a coupling agent and a silicon-based agent. [0003] Propyltrimethoxysilane, the raw material for synthesizing acidic crosslinking agent, is prepared from the by-product of γ-chloropropyltrimethoxysilane. γ-chloropropyltrime...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 刘明峰吴兵兵黄贻萍陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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