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Preparation method of novel isocyanate-based silane

A technology of isocyanate and ester-based alkoxysilane is applied in the field of preparation of novel isocyanate-based silane, and achieves the effect of high catalytic efficiency and strong selectivity

Inactive Publication Date: 2017-03-08
山东禹王和天下新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, there is currently no method for the preparation of isocyanate-based silanes that is technically feasible, simple and efficient, and easy to promote.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0011] A kind of preparation method of novel isocyanatosilane, comprises steps as follows:

[0012] (1) Aminoalkoxysilane reacts with dialkyl carbonate at a temperature of 30°C to 80°C to form carbamate-based alkoxysilane;

[0013] (2) The urethane-based alkoxysilane is cracked under the catalysis of the catalyst to generate isocyanate-based silane.

[0014] Preferably in the present invention, the mass ratio of aminoalkoxysilane to dialkyl carbonate in step (1) is: (9-15): (6-12), and the reaction time is 0.5-3h.

[0015] Preferably in the present invention, the specific preparation steps of step (1) carbamate alkoxysilane are as follows:

[0016] Add dimethyl carbonate to the methanol solution of sodium methylate under magnetic stirring and stir evenly, then add aminomethylmethyldimethoxysilane dropwise, the mass ratio of aminoalkoxysilane to dialkyl carbonate is: ( 9~15): (6~12), after the dropwise addition, the temperature is raised to 50°C~70°C, and the reaction time is...

specific Embodiment approach

[0034] The present invention will be further described below in conjunction with the examples, but not limited thereto.

[0035] A kind of preparation method of novel isocyanatosilane, comprises steps as follows:

[0036] (1) Preparation of carbamate silane:

[0037] Add 90g of dimethyl carbonate to a 500ml four-necked flask with magnetic stirring, add 2g of 30% methanol solution of sodium methoxide, and then drop 135g of aminomethylmethyldimethoxysilane into the four-necked flask within 30min , the reaction temperature was controlled at 30°C. After the dropwise addition, the temperature was raised to 70° C., and the reaction was continued for 1 h. The product was neutralized with ammonium chloride in methanol, filtered, and the resulting filtrate was distilled under reduced pressure to obtain 185 g of the product, with a yield of 95.8%.

[0038] (2) Preparation of isocyanate silane

[0039] Tin-containing molecular sieve raw powder a:

[0040] a) Dissolve 30g CTAB in 200g...

Embodiment 2

[0049] A kind of preparation method of novel isocyanatosilane, comprises steps as follows:

[0050] (1) Preparation of carbamate silane:

[0051] Add 90g of dimethyl carbonate to a 500ml four-necked flask with magnetic stirring, add 2g of 30% methanol solution of sodium methoxide, and then drop 135g of aminomethylmethyldimethoxysilane into the four-necked flask within 30min , the reaction temperature was controlled at 30°C. After the dropwise addition, the temperature was raised to 70° C., and the reaction was continued for 1 h. The product was neutralized with ammonium chloride in methanol, filtered, and the resulting filtrate was distilled under reduced pressure to obtain 185 g of the product, with a yield of 95.8%.

[0052] (2) Preparation of isocyanate silane

[0053] Tin-containing molecular sieve raw powder b:

[0054] a) Dissolve 15g CTAB in 150g deionized water for use.

[0055] b) Dissolve 8.5g NaOH in 20g deionized water for later use.

[0056] c) 71.6g SnCl22H2O ...

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PUM

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Abstract

The invention relates to a preparation method of novel isocyanate-based silane. The method comprises steps as follows: (1) aminoalkoxy silane and dialkyl carbonate react at the temperature of 30-80 DEG C to produce carbamate-based alkoxy silane; (2) carbamate-based alkoxy silane is split under the catalysis of a catalyst to produce isocyanate-based silane. Prepared isocyanate-based silane can greatly reduce the resin viscosity, thus, more filler can be added, the glue mixing cost is reduced, meanwhile, the mechanical property is improved, the resin activity is improved, and the dosage of tin catalysts is reduced. The selectivity of the used catalysts is high, the raw material conversion rate is high, and the product yield is high.

Description

technical field [0001] The invention relates to a preparation method of a novel isocyanate-based silane, which belongs to the technical field of compound synthesis. Background technique [0002] Silane-crosslinked adhesives and sealants include alkoxysilane-terminated polymers as adhesives. Polymer systems with reactive alkoxysilyl groups have long been known. However, most of the silane-terminated resin materials on the market are gamma-terminated. This type of resin has low activity and requires the use of toxic tin compounds for curing. catalyst. α-silane-terminated resins have higher activity and can be cross-linked and cured well without tin catalysts. However, due to technical reasons, α-silanes cannot be mass-produced, and α-silanes cannot be purchased in the market. [0003] The preparation of α-type silane also has some public reports in patent documents, such as: U.S. patent document US5393910 discloses a method for generating isocyanatosilane by pyrolysis of ure...

Claims

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Application Information

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IPC IPC(8): C07F7/18B01J31/26
CPCC07F7/1892B01J31/26
Inventor 孙清松
Owner 山东禹王和天下新材料有限公司
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