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The synthetic method of 3-mercaptopropyltriethoxysilane

A technology of mercaptopropyltriethoxysilane and chloropropyltriethoxysilane, which is applied in the field of synthesis of 3-mercaptopropyltriethoxysilane, can solve the problem of harsh reaction conditions, strong odor of guanidine salt, Large production safety hazards and other problems, to achieve the effect of high product yield and purity, mild reaction conditions, and short production cycle

Active Publication Date: 2017-10-31
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages are: the raw material 3-chloropropyltriethoxysilane needs to be neutralized, which increases the operating procedures; the reaction raw materials and equipment are required to be anhydrous, and the reaction conditions are relatively harsh; the by-product with a large output is guanidine salt odor Strong smell, serious environmental pollution
The disadvantage is that the hydrogen sulfide used is a highly toxic gas, which needs to be carried out under high pressure, which has great hidden dangers in production safety and high requirements for production equipment.
Although this patent reports that this method has a product yield of 85% to 95%, when the patentee adopts this method to prepare 3-mercaptopropyltriethoxysilane, he finds that many side effects such as silane hydrolysis, condensation, and coagulation are generated. The white gel formed by the reaction, the color of the prepared product is slightly light yellow, and the yield is only about 50%

Method used

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  • The synthetic method of 3-mercaptopropyltriethoxysilane
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  • The synthetic method of 3-mercaptopropyltriethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of synthetic method of 3-mercaptopropyltriethoxysilane realizes, and this method comprises the following steps:

[0036] Step 1: Take 75mL of distilled water and heat it to 40°C, dissolve 47.5g of sodium monohydrogen phosphate and 2.5g of sodium dihydrogen phosphate in the distilled water to obtain a buffer solution;

[0037] Step 2, add 2.73g of potassium iodide and 75g of sodium hydrosulfide to the buffer solution, stir and heat up to 75°C;

[0038] Step 3: After adding 7.27g of tetrabutylammonium bromide to dissolve for 5min, add 115g of 3-chloropropyltriethoxysilane within 10min, and stop the reaction after stirring for 1.5h to obtain a reaction solution;

[0039] Step 4. After separating the reaction liquid, take the upper layer liquid and filter it in an ice bath for 30 minutes to obtain the crude product of 3-mercaptopropyltriethoxysilane, and then carry out vacuum distillation to obtain the 3-mercaptopropyl Triethoxysilane.

Embodiment 2

[0041] A kind of synthetic method of 3-mercaptopropyltriethoxysilane realizes, and this method comprises the following steps:

[0042] Step 1: Take 80 mL of distilled water and heat it to 47°C, and dissolve 47.5 g of sodium monohydrogen phosphate and 2.5 g of sodium dihydrogen phosphate in the distilled water to obtain a buffer solution;

[0043] Step 2, add 2.5g of potassium iodide and 78.56g of sodium hydrosulfide to the buffer solution, stir and heat up to 87°C;

[0044] Step 3: After adding 7.5 g of tetrabutylammonium bromide and dissolving for 5 min, add 120 g of 3-chloropropyltriethoxysilane within 10 min, and stop the reaction after stirring for 1.5 h to obtain a reaction solution;

[0045] Step 4. After separating the reaction liquid, take the upper layer liquid and filter it in an ice bath for 30 minutes to obtain the crude product of 3-mercaptopropyltriethoxysilane, and then carry out vacuum distillation to obtain the 3-mercaptopropyl Triethoxysilane.

Embodiment 3

[0047] A kind of synthetic method of 3-mercaptopropyltriethoxysilane realizes, and this method comprises the following steps:

[0048] Step 1: Take 100 mL of distilled water and heat it to 50° C., dissolve 47.5 g of sodium monohydrogen phosphate and 2.5 g of sodium dihydrogen phosphate in the distilled water to obtain a buffer solution;

[0049] Step 2, add 1.875g of potassium iodide and 80g of sodium hydrosulfide to the buffer solution, stir and heat up to 100°C;

[0050] Step 3: After adding 8.125 g of tetrabutylammonium bromide and dissolving for 5 minutes, add 125 g of 3-chloropropyltriethoxysilane within 10 minutes, and stop the reaction after stirring for 1.5 hours to obtain a reaction liquid;

[0051] Step 4. After separating the reaction liquid, take the upper layer liquid and filter it in an ice bath for 30 minutes to obtain the crude product of 3-mercaptopropyltriethoxysilane, and then carry out vacuum distillation to obtain the 3-mercaptopropyl Triethoxysilane.

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Abstract

The invention discloses a synthesizing method of 3-mercaptopropyltriethoxysilane. A mass ratio of catalyst potassium iodide to tetrabutylammonium bromide is 3:8-13 in the process of taking sodium hydrosulfide and 3-chloropropyltriethoxysilane as raw materials to synthesize 3-mercaptopropyltriethoxysilane. The synthesizing method is simple in synthesizing process, convenient in operation, short in production period, light in odor, high in yield, safe and environment friendly.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing 3-mercaptopropyltriethoxysilane. Background technique [0002] 3-Mercaptopropyltriethoxysilane is an additive that can improve the adhesion between inorganic substances and organic substances. The hydrolysis of functional groups to generate silanols can interact with inorganic substances, thereby firmly bonding organic polymers and inorganic fillers together. Therefore, 3-mercaptopropyltriethoxysilane is often used to treat inorganic fillers such as silica and carbon black, and to act as an active agent, coupling agent, crosslinking agent or supplementary agent in polymers such as rubber and silicone rubber. The role of strong agents. On the other hand, 3-mercaptopropyltriethoxysilane can be filled with resins, elastomers, fibers, metals, minerals, glass, etc. to improve the mechanical and electrical properties of the system. Filling 3-mercaptopropylt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 钟伟王宏丹刘小明
Owner JIAXING UNIV