Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method capable of increasing content and yield of gamma-chloropropyltriethoxysilane simultaneously

A technology of chloropropyltriethoxysilane and content, which is applied in the field of increasing the content and yield of γ-chloropropyltriethoxysilane at the same time, which can solve the high requirements of process control and automation level and the difficulty of unit operation technology , large investment in production equipment and other issues, to achieve the effects of short heating time, reduced construction investment, and fast distillation speed

Inactive Publication Date: 2010-02-17
青岛荣达新材料研究所
View PDF0 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Secondly, the direct method that has just entered trial production uses silicon powder and ethanol as the main raw materials to first synthesize triethoxysilane and then react with chloropropene to synthesize γ-chloropropyltriethoxysilane; the existing production processes mainly include the following Disadvantages: (1) The finished product content is low, generally at 98.5%, rarely more than 99%, and the product above 99.5% is even less; (2) The impurity content is high, and the free chlorine content in the product is high, which is used in the production of special catalyst carriers , aerospace materials, preparation of ionic liquid catalysts, and production of special-purpose rubber products are more restricted
Although the direct method has the advantages of shortening the synthesis steps, reducing production costs, not releasing hydrogen chloride, avoiding environmental pollution, and improving product quality, it still has the following disadvantages: 1. The quality requirements for raw materials, especially silicon powder, are extremely strict, including content, particle size, Iron medium content and other indicators; ②High requirements for process control and automation level, difficult unit operation technology; ③Large investment in production equipment; ④High technical difficulty

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1 The esterification reaction is carried out in a 2000L kettle

[0024] (1) Take by weighing 1100 grams of lithium chloride, 800 grams of 4-dimethylaminopyridine, and 1000 grams of aliphatic alkyl dimethyl tertiary amines, respectively add in 4500 milliliters of absolute ethanol, and fully mix them in a glass container, Sealed and ready for use.

[0025] (2) Measure 800Kg gamma-chloropropyl trichlorosilane into the reactor; measure 2800 ml of absolute ethanol solution containing lithium chloride into the reactor, measure 3000 ml of anhydrous ethanol containing 4-dimethylaminopyridine The ethanol solution is added to the esterification kettle.

[0026] (3) 650Kg absolute ethanol is measured for subsequent use.

[0027] (4) Add absolute ethanol to the esterification kettle, control the reaction temperature at 45-50°C, pay close attention to the working conditions of the hydrogen chloride recovery system, adjust the flow rate, temperature and vacuum of the system in time...

Embodiment 2

[0041] 1 The esterification reaction is carried out in a 2000L kettle

[0042] (1) Weigh 1250 grams of lithium chloride, 750 grams of 4-dimethylaminopyridine, and 1300 grams of aliphatic alkyl dimethyl tertiary amines respectively, add them to 4000 milliliters of absolute ethanol respectively, and place them on glass, glass-lined or PVC material In a container, mix well and seal well for later use.

[0043] (2) Measure 850Kg gamma-chloropropyl trichlorosilane into the reactor; measure 2900 ml of absolute ethanol containing lithium chloride into the reactor, measure 3100 ml of anhydrous ethanol containing 4-dimethylaminopyridine The ethanol solution is added to the esterification kettle.

[0044] (3) Pump the measured 675Kg absolute ethanol into the head tank.

[0045] (4) Add absolute ethanol to the esterification kettle, control the reaction temperature at 45-48°C, pay close attention to the working conditions of the hydrogen chloride recovery system, adjust the flow rate, ...

Embodiment 3

[0058] 1 The esterification reaction is carried out in a 2000L kettle

[0059] (1) Weigh 1400 grams of lithium chloride, 850 grams of 4-dimethylaminopyridine, and 1300 grams of fatty alkyl dimethyl tertiary amine respectively, add them to 4000 milliliters of absolute ethanol respectively, and place them on glass, glass-lined or PVC material In a container, mix well and seal well for later use.

[0060] (2) Measure 900Kg γ-chloropropyl trichlorosilane into the reactor; measure 2950 milliliters of absolute ethanol containing lithium chloride and add it to the reactor, measure 3300 milliliters of anhydrous ethanol containing 4-dimethylaminopyridine The ethanol solution was added to the reaction kettle.

[0061] (3) Pump the measured 740Kg absolute ethanol into the head tank.

[0062] (4) Add absolute ethanol to the esterification kettle, control the reaction temperature at 45-50°C, pay close attention to the working conditions of the hydrogen chloride recovery system, adjust th...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method capable of increasing the content and yield of gamma-chloropropyltriethoxysilane simultaneously, and the method comprises the following steps: adopting gamma-chloropropyltrichlorosilane prepared by the reaction of trichlorosilane and chloropropene to react with ethanol and finally obtaining gamma-chloropropyltriethoxysilane though esterification, neutralization anddistillation. The invention adds lithium chloride, 4-methylaminopyridine and fatty alkyl dimethyl tertiary amine as esterifying catalyst in esterification reaction for the synergetic catalysis to thereaction between gamma-chloropropyltrichlorosilane and ethanol so as to increase the product content, greatly increase the conversion rate of gamma-chloropropyltrichlorosilane, increase the product yield, inhibit the side effect, shorten the reaction time, reduce the impurity content of the product and reduce the Cl<-> content in the product of which target value is not more than 50ppm.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for simultaneously increasing the content and yield of γ-chloropropyltriethoxysilane. Background technique [0002] Due to its unique good performance, silane coupling agent can form a firm bond between inorganic materials and organic materials, enhance the mechanical properties, electrical properties, water resistance, etc. of materials, and is widely used in glass fiber and radial tires. The use of silane coupling agents in glass fibers accounts for about 50% of the total domestic consumption of silane coupling agents; the second is radial tires, accounting for more than 40%, and the rest is used in consumer fields such as coatings. With the development of glass fiber industry and radial tire industry, it is expected that during the Eleventh Five-Year Plan period, the demand for silane coupling agents in my country will maintain a growth rate of more than 10%. With t...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/20B01J31/26B01J31/02
Inventor 张中法黄慧郭学阳吕彩玲丁爱梅张庆国张志刚
Owner 青岛荣达新材料研究所
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products