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Synthesizing method of gamma-aminopropyl triethoxysilane

The technology of aminopropyltriethoxysilane and chloropropyltriethoxysilane is applied in the synthesis field of γ-aminopropyltriethoxysilane, which can solve the problem of high impurity content in products and achieve the impurity content of products. Low, the production operation safety is improved, the effect of saving steam

Inactive Publication Date: 2012-05-30
青岛惠国新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a synthetic method of γ-aminopropyltriethoxysilane to solve the problem of high impurity content in the product existing in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Amination reaction

[0032] (1) Weigh 5.7 kg of aluminum isopropoxide and 2.8 kg of phenyldiethanolamine respectively, add them into 705 kg of toluene, stir and mix well in an anhydrous reaction kettle, prepare a solvent solution and seal it for later use.

[0033] (2) Under vacuum conditions, the solvent solution prepared above and 920 kilograms of γ-chloropropyltriethoxysilane are added to an anhydrous reactor, and 465 kilograms of ammonia are added under stirring, and the contents of the reactor are The temperature was raised to 62°C, the reaction pressure was 2.3 MPa, and the reaction was carried out for 5.5 hours.

[0034] 2. Filtration and separation

[0035] When the material temperature in the reactor has a downward trend, cool down to 50°C. Open the pressure relief valve to recover the unreacted ammonia and make it into concentrated ammonia water to produce other products. Use compressed air to press the material in the reactor to the tank filter to filte...

Embodiment 2

[0042] 1 amination

[0043] (1) Weigh 6.3 kg of aluminum isopropoxide and 3.1 kg of phenyldiethanolamine respectively, add them into 735 kg of toluene, stir and mix well in an anhydrous reactor, prepare a solvent solution and seal it for later use.

[0044] (2) Under vacuum conditions, the above-mentioned prepared solvent solution and 950 kg of γ-chloropropyltriethoxysilane are added to the anhydrous reactor, and 490 kg of ammonia are added under stirring, and the contents of the reactor are Slowly raise the temperature to 61°C, control the reaction pressure to 2.4MPa, and react for 5h.

[0045] 2. Filtration and separation

[0046] When the material temperature in the reactor has a downward trend, cool down to 50°C. Open the pressure relief valve to recover the unreacted ammonia and make it into concentrated ammonia water to produce other products. Use compressed air to press the material in the reactor to the tank filter to filter out the generated NH 4 Cl, NH 4 Cl is p...

Embodiment 3

[0053] 1 amination

[0054] (1) Weigh 6.95 kilograms of aluminum isopropoxide and 3.4 kilograms of phenyldiethanolamine respectively, add them into 750 kilograms of toluene, stir and mix well in an anhydrous reaction kettle, prepare a solvent solution and seal it for later use.

[0055] (2) Under vacuum conditions, the above-mentioned prepared solvent solution and 980 kg of γ-chloropropyltriethoxysilane are added to the anhydrous reactor, and 505 kg of ammonia are added under stirring, and the contents of the reactor are Slowly raise the temperature to 65°C, control the reaction pressure to 2.8MPa, and react for 6h.

[0056] 2. Filtration and separation

[0057] When the material temperature in the reactor has a downward trend, cool down to 50°C. Open the pressure relief valve to recover the unreacted ammonia and make it into concentrated ammonia water to produce other products. Use compressed air to press the material in the reactor to the tank filter to filter out the gen...

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PUM

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Abstract

The invention discloses a synthesizing method of gamma-aminopropyl triethoxysilane, comprising the following steps of: (1) adding a toluene solution dissolved with a catalyst and the gamma-aminopropyl triethoxysilane to a reaction still under the condition of vacuum, adding ammonia in a stirring state, and increasing the temperature of materials inside the reaction still to 60-70 DEG C to react for 4-7 hours at the reaction pressure of 0.5-3 MPa; (2) after amination reaction is finished, filtering, separating and removing side products, and adding filter liquor to a distilling still; (3) after the top temperature of the distilling still is more than or equal to 102 DEG C, reducing the temperature of the materials inside the distilling still to be less than or equal to 80 DEG C, and carrying out reduced pressure distillation at vacuum degree of more than or equal to 0.099 MPa so as to obtain the gamma-aminopropyl triethoxysilane after the reduced pressure distillation. The invention enhances the purity of synthesized products by more than 99 percent (GC) and expands the application fields to industries, i.e. electronic and electric products, high-performance catalyst preparation, nanometer materials, superfine dispersing materials, and the like which have higher requirements for product purity.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of γ-aminopropyltriethoxysilane. Background technique [0002] γ-Aminopropyltriethoxysilane (hereinafter referred to as KH-550) is an important aminohydrocarbylsilane with two functional groups, amino and ethoxy. Three of the hydrolyzable groups (ethoxyl groups) are first hydrolyzed to form silanols in the reaction. Since silanols are unstable, they are very easy to combine with the hydroxyl groups on the surface of inorganic substances or metals for dehydration, thereby combining with inorganic substances or metals. There are two active hydrogens on the amino group, which can react with various polymers, so that two materials with completely different properties can be closely combined through chemical bonds. KH-550 has a wide range of uses. It can be used as an excellent glass fiber treatment agent, an excellent adhesion promoter, and a filler additive for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C07F7/20
Inventor 张中法
Owner 青岛惠国新材料科技有限公司
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