Synthesis method of mixing ketoxime type cross-linking agent

A synthesis method and cross-linking agent technology, which is applied in the field of synthesis of mixed ketoxime cross-linking agents, can solve the problems of cumbersome synthesis process, poor color stability, long synthesis time, etc., and achieve simple precipitation and separation, easy separation and simple operation Effect

Active Publication Date: 2012-07-25
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

3. The synthesis process of the mixture of methyl tributyl ketoxime silane and other ketoxime crosslinking agents is cumbersome, the synthesis time is long, and the cost is high
4. Silicone ru

Method used

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  • Synthesis method of mixing ketoxime type cross-linking agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 808 g of butanone oxime and 273.1 g of industrial heptane into a 2000 ml three-necked reaction flask, and add 273.1 g of a mixture of propyltrichlorosilane and phenyltrichlorosilane dropwise under stirring at 300 rpm. Among them, 1.3mol of propyl trichlorosilane, 230.8g in total; 0.2mol of phenyltrichlorosilane, 42.3g in total, the temperature is controlled at 25°C, and the dropping time is controlled at 3 hours; after the dropping is completed, continue to react for 1 hour to generate propylene A mixture of phenyltributanoximinosilane and phenyltributanoximinosilane. After the reaction, the mixture was left to stand for 8 hours, and the mixture system was divided into two distinct upper and lower layers. The upper layer was the crude product of propyl tributylketoxime silane and phenyl tributylketoxime silane, and the lower layer was butanone oxime hydrochloride. . After the stratification is completed, the butanone oxime hydrochloride in the lower layer is separa...

Embodiment 2

[0026] Put 808g of butanone oxime and 273.1g of industrial heptane into a 2000ml three-necked reaction flask, and add 273.1g of propyltrichlorosilane and phenyltrichlorosilane mixture dropwise under stirring at 250 rpm; wherein 1.3 propyltrichlorosilane mol, 230.8g in total, 0.2 mol of phenyltrichlorosilane, 42.3g in total. During the reaction process, the temperature was controlled at 35° C., and the dropwise addition time was controlled at 2 hours. After the dropwise addition was completed, the reaction was continued for 1 hour to generate a mixture of propyl tributylketoxime silane and phenyl tributylketoxime silane. After the reaction, the mixture was left to stand for 10 hours, and the mixture system was divided into two distinct upper and lower layers. The upper layer was the crude product of propyl tributylketoxime silane and phenyl tributylketoxime silane, and the lower layer was butanone oxime hydrochloride. . After the stratification is completed, after separating ...

Embodiment 3

[0028] 808g of butanone oxime and 273.1g of industrial heptane were dropped into a 2000ml three-necked reaction flask, and 273.1g of propyltrichlorosilane and phenyltrichlorosilane mixture were added dropwise under stirring at 300 rpm; wherein propyltrichlorosilane 1.3 mol, 230.8g in total, 0.2 mol of phenyltrichlorosilane, 42.3g in total. During the reaction process, the temperature was controlled at 40° C., and the dropwise addition time was controlled at 1 hour. After the dropwise addition was completed, the reaction was continued for 1 hour to generate a mixture of propyl tributylketoxime silane and phenyl tributylketoxime silane. After the reaction, the mixture was left to stand for 9 hours, and the mixture system was divided into two obvious upper and lower layers. The upper layer was the crude product of propyl tributylketoxime silane and phenyl tributylketoxime silane, and the lower layer was butanone oxime hydrochloride . After the stratification is completed, after...

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Abstract

The invention relates to a synthesis method of a mixed ketoxime type cross-linking agent, belonging to the field of silane cross-linking agent synthesis. The synthesis method comprises the steps: reacting propyl trichlorosilane, phenyl trichlorosilane and diacetylmonoxime as raw materials to generate a mixture of propyl tri-diacetylmonoxime silane (ProS) and phenyl tri-diacetylmonoxime silane (PhOS); and after reaction is finished, standing and layering, removing lower-layer diacetylmonoxime hydrochloride, introducing ammonia gas to the upper-layer half-finished product for neutralizing, filtering to remove white solid ammonium chloride, and then distilling to obtain the mixed ketoxime type cross-linking agent. According to the invention, the ratio of PrOS to PhOS in the mixed cross-linking agent can be accurately controlled according to the use requirement of the cross-linking agent; and the synthesis method has the advantages of simplicity in operation, stable quality, high reactionconversion rate, high yield, low diacetylmonoxime consumption, low production cost and the like; and the whole process has no wastewater generation and has no environmental pollution.

Description

technical field [0001] The invention relates to a synthesis method of a mixed ketoxime type crosslinking agent, belonging to the field of synthesis of silane crosslinking agents. Background technique [0002] A cross-linking agent is a substance that can act as a bridge between linear molecules, allowing multiple linear molecules to bond and cross-link each other to form a network structure. The cross-linking agent is mainly used in polymer materials (rubber and thermosetting resin), and its function is to generate chemical bonds between the linear molecules, so that the linear molecules are connected together to form a network structure, which can improve the strength of the rubber, Elasticity, heat resistance, wear resistance, solvent resistance and other properties. [0003] Ketoximosilane is currently the most used crosslinking agent in the market, and it is also the fastest growing category in the Chinese market in recent years. Methyl tributylketoxime silane (MOS), v...

Claims

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Application Information

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IPC IPC(8): C08K5/5465C07F7/10
Inventor 王欣阮少阳王灿胡江华汤艳甘俊陈圣云
Owner JINGZHOU JIANGHAN FINE CHEM
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