Synthesis method of gamma-aminopropyl triethoxy silane

A technology of aminopropyltriethoxysilane and chloropropyltriethoxysilane, which is applied in the field of synthesis of γ-aminopropyltriethoxysilane, can solve the complex post-processing process, the potential safety hazard, the increased problems such as preparation costs, to avoid excessive consumption, shorten the reaction time, and reduce the amount of use

Inactive Publication Date: 2021-01-19
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of preparation method not only has a long reaction time, but also causes complicated post-treatment process due to the excessive amount of ammonia gas
At the same time, ammonia gas needs to be discharged, which not only has potential safety hazards, but also increases the preparation cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of synthetic method of γ-aminopropyltriethoxysilane provided by the present invention comprises the following steps:

[0029] Step 1, first add ammonia water to the reactor, and add the buffer agent according to the molar ratio of ammonia water (calculated as ammonia):buffer agent is 3-5:1-2;

[0030] Step 2, install a condensing reflux device and raise the temperature to 70°C to 85°C;

[0031] Step 3, according to the molar ratio of ammonia water (calculated as ammonia):phase transfer catalyst:buffering agent is 3~5:0.01:1~2, add buffering agent and phase transfer catalyst, and stir for about 10min~20min;

[0032] Step 4, according to the molar ratio of 3-chloropropyltriethoxysilane:ammonia water (calculated as ammonia):phase transfer catalyst:buffering agent is 1:3~5:0.01:1~2, drop into 3-chloropropane Triethoxysilane;

[0033] Step 5, carry out ammonolysis reaction after the dropwise addition, the ammonolysis reaction temperature is 70°C-100°C, and the heat ...

Embodiment 2

[0039] A kind of synthetic method of γ-aminopropyltriethoxysilane provided by the present invention comprises the following steps:

[0040] Step 1, first add ammonia water to the reactor, according to the molar ratio of ammonia water (calculated as ammonia): buffering agent is added in the ratio of 4:1.5;

[0041] Step 2, install a condensing reflux device and raise the temperature to 70°C to 85°C;

[0042] Step 3, according to the molar ratio of ammonia water (calculated as ammonia):phase transfer catalyst:buffering agent is 4:0.01:1.5, add buffering agent, add phase transfer catalyst, and stir for about 12min to 15min;

[0043] Step 4, according to the molar ratio of 3-chloropropyltriethoxysilane: ammoniacal liquor (calculated as ammonia): phase transfer catalyst: buffering agent is the ratio of 1:4:0.01:1.5 to drop 3-chloropropyltriethoxy 3-Chloropropyltriethoxysilane and 3-chloropropyltriethoxysilane are added dropwise within 50 minutes to 55 minutes, and the temperature ...

Embodiment 3

[0049] Step 1, adding 347g of ammonia water with a mass fraction of 10% in a 1000mL flask reactor, and then adding 125.85g of anhydrous trisodium phosphate;

[0050] Step 2, install a condensing reflux device, and slowly raise the temperature to a system temperature of 80°C;

[0051]Step 3, add 1.6g tetrabutylammonium bromide, stir for about 10min;

[0052] Step 4, add 123g of 3-chloropropyltriethoxysilane dropwise, the dropwise addition is completed in 60 minutes, and the temperature is controlled not to exceed 85°C during the dropwise addition;

[0053] Step 5, carry out the ammonolysis reaction after the dropwise addition, the ammonolysis reaction temperature is 80°C, and the heat preservation reaction time is 3.5h;

[0054] Step 6: After the ammonolysis reaction is completed, liquid separation is carried out, and the supernatant liquid is taken for suction filtration and dehydration post-treatment to finally obtain γ-aminopropyltriethoxysilane. The present invention fina...

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PUM

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Abstract

The invention discloses a synthesis method of gamma aminopropyl triethoxy silane, belongs to the technical field of organic silicon synthesis, and particularly relates to a synthesis method of gamma aminopropyl triethoxy silane. The method is characterized in that 3-chloropropyltriethoxysilane and ammonia water are used as reaction substrates, and ammonolysis reaction is performed according to themolar ratio of 3-chloropropyltriethoxysilane to ammonia water (calculated by ammonia) to a phase transfer catalyst to a buffer agent being 1: (3-5): 0.01: (1-2) to prepare gamma aminopropyltriethoxysilane. The invention has the advantages that the reaction time is shortened, and the product yield is increased; and meanwhile, the use amount of ammonia gas is reduced, the product purity is high, the post-treatment process is simple, and the method is green and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of organosilicon synthesis, in particular to a synthesis method of gamma-aminopropyltriethoxysilane. Background technique [0002] Silane coupling agents are widely used in automotive, aviation, medical, construction, electronics and other fields. At present, γ-aminopropyltriethoxysilane is generally prepared by ammonolysis reaction under high pressure with 50 times the molar amount of ammonia gas and 1 times the molar amount of 3-chloropropyltriethoxysilane. This preparation method not only has a long reaction time, but also causes complicated post-treatment processes due to excessive ammonia gas. At the same time, ammonia gas needs to be discharged, which not only has potential safety hazards, but also increases the preparation cost. Contents of the invention [0003] The object of the present invention is to provide a synthesis method of γ-aminopropyltriethoxysilane, so as to achieve the purpose of sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1876C07F7/1804
Inventor 王庆振马松潘琳琳冉升亮吴彩英苏冉刘建元张新杜嘉乐
Owner SHANDONG YANGGU HUATAI CHEM
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