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Prepn of isocyanate-containing alkyl silane or alkyl siloxane

A technology of cyanate alkoxysilane and isocyanate alkylsilane, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve complex reaction process operations, pollute the environment, Low safety and other issues, to achieve the effect of simple process route, cheap and easy-to-obtain raw materials, and high reaction selectivity

Inactive Publication Date: 2007-01-03
湖北德邦化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the above several methods, what the phosgene method adopted was the reaction of gaseous phosgene and liquid aminohydrocarbyl silane, although the reaction can be realized, the operation of the gas-liquid reaction process is complicated and the safety is low; In the method adopted, the reaction needs to be cracked at high temperature (100-260° C.) with the help of an alkali metal organic salt as a catalyst to prepare isocyanate alkyl alkoxysilane. Therefore, the reaction conditions are harsh; the alkali metal isocyanate method adopts The raw material sodium isocyanate or potassium salt is very toxic, which brings inconvenience to production and research, and pollutes the environment at the same time

Method used

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  • Prepn of isocyanate-containing alkyl silane or alkyl siloxane
  • Prepn of isocyanate-containing alkyl silane or alkyl siloxane
  • Prepn of isocyanate-containing alkyl silane or alkyl siloxane

Examples

Experimental program
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Effect test

example 1

[0049] Example one, the synthesis of isocyanate propyltriethoxysilane:

[0050] 1. Dissolve 20 grams of bis(trichloromethyl)carbonate into 150ML of tetrahydrofuran solution and add it to the constant pressure dropping funnel A;

[0051] 2 Add 44 grams of aminopropyltriethoxysilane and 70 grams of pyridine to 60 mL of tetrahydrofuran into the constant pressure dropping funnel B;

[0052] 3. At 0°C ~ 5°C, slowly drop the mixture of A and B into a 500ml four-neck flask respectively, after 2 hours, continue to react at 0°C for 2 hours;

[0053] 4. Raise the temperature to 65°C for 1 hour;

[0054] 5. Reduce to room temperature, filter and remove tetrahydrofuran;

[0055] 6. Finally, bp 130°C / 20mmHg, distilled under reduced pressure to obtain isocyanate propyltriethoxysilane product, 36.6g, with a yield of 70% and a product content of 98.15%.

[0056] Product is analyzed by gas chromatography: product purity 98.15%; FT-IR infrared spectrometer and 1 H-NMR mass spectrometry anal...

Embodiment 2

[0057] Embodiment two, the synthesis of isocyanate propylmethyldiethoxysilane:

[0058] 1. Dissolve 20 grams of bis(trichloromethyl)carbonate into 150ML of tetrahydrofuran solution and add it to the constant pressure dropping funnel A;

[0059] 2. Add 38.2 g of aminopropylmethyldiethoxysilane, 70 g of pyridine and 80 mL of tetrahydrofuran into the constant pressure dropping funnel B;

[0060] 3. At -5°C to 0°C, slowly drop the mixtures of A and B into a 500ml four-neck flask respectively, and the dropwise addition is completed in 2 hours, then continue to react at -5°C to 0°C for 2 hours;

[0061] 4 Heat up to 60°C for 1 hour

[0062] 5. Reduce to room temperature, filter and remove tetrahydrofuran;

[0063] 6. Finally, 29.50 g of isocyanate propylmethyldiethoxysilane was obtained by vacuum distillation at bp91-93°C / 9mmHg, with a yield of 68% and a content of 97.60%.

[0064] The product is analyzed by gas chromatography: product purity 97.60%; FT-IR infrared spectrometer a...

Embodiment 3

[0065] Embodiment three, the synthesis of isocyanate propyltriethoxysilane:

[0066] 1. Dissolve 20 grams of bis(trichloromethyl)carbonate and 150ML of toluene solution into the constant pressure dropping funnel A;

[0067] 2. Add 44 grams of aminopropyltriethoxysilane and 50 grams of dimethylaniline to 60ML of toluene into the constant pressure dropping funnel B;

[0068] 3. At 0°C ~ 5°C, slowly drop the mixture of A and B into a 500ml four-neck flask respectively, after 2 hours, continue to react at 0°C for 2 hours;

[0069] 4. Raise the temperature to 65°C for 1 hour;

[0070] 5. Cool down to room temperature, filter and remove toluene;

[0071] 6. Finally, bp 130°C / 20mmHg vacuum distillation to obtain isocyanate propyltriethoxysilane product, 31.47g, yield 64%, product content 97.92%.

[0072] Product is analyzed by gas chromatography: product purity 97.92%; FT-IR infrared spectrometer and 1 H-NMR mass spectrometry analysis and characterization: at 2272cm-1 is the char...

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Abstract

The process of preparing isocyanate containing alkyl silane or alkyl siloxane includes the following steps: 1. dissolving bis(trichloromethyl) carbonate in inert organic solvent through stirring and adding the solution into dropping pot I; 2. mixing primary amine alkyl silane or amino alkoxy silane, tertiary amine compound and inert organic solvent in the mass ratio of 1 to 1.5-6 to 2-5, and adding the mixture into dropping pot II; cooling the main reaction kettle to -30 deg.c to 30 deg.c, dropping the solution and the mixture into the main reaction kettle and further stirring for reaction; 4. heating the reacted solution in one other reactor, heating to 50-100 for further reaction of 2-4 hr until no primary amine may be detected; 5, high speed centrifugally filtering the reacted mixture; and 6. distilling in a distiller to eliminate solvent and decompression rectifying.

Description

technical field [0001] The present invention relates to the preparation method of isocyanate-containing alkylsilane or isocyanate alkoxysilane, especially the method of producing isocyanate-containing alkylsilane or isocyanate alkoxysilane by bis(trichloromethyl)carbonate method. Isocyanate-containing alkylsilane or isocyanate alkoxysilane is mainly used to treat the surface of inorganic, organic and metal materials, endowing them with good adhesion between different materials. Background technique [0002] Isocyanate alkyl silane or isocyanate alkoxy silane is mainly used to treat the surface of inorganic, organic and metal materials, endow them with good adhesion to dissimilar materials, and improve the overall performance of materials or products; it can be used with amines, laminates Reaction of hydrogen nitride and phosphate ester to obtain corresponding silane coupling agent containing urea group, azide group and phosphate ester group; used as a tackifier for room temp...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 张群朝王德才刘胜王新建
Owner 湖北德邦化工新材料有限公司
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