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Synthesis method of isocyanate curing agent

An isocyanate and synthesis method technology, applied in polyurea/polyurethane coatings, coatings, fire-retardant coatings, etc., can solve the problems of less obvious coupling effect, insufficient cross-linking strength of paint film, and short operating time, etc. Large market prospects and economic value, speed controllable, and the effect of improving high temperature resistance

Inactive Publication Date: 2017-05-10
SHENZHEN FEIYANG JUNYAN TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem in the application of siloxane coupling agents produced under the existing technology in the polyurethane coating industry is that if aminopropyltriethoxysilane is added, due to the strong activity of primary amines, the reaction with isocyanate is too fast and the operating time is too short; However, if a coupling agent with epoxy groups is added, the effect of coupling is not obvious because the epoxy groups do not react with isocyanate; if monofunctional isocyanate siloxane is added, the crosslinking strength of the paint film is insufficient, There will be stickiness of the paint film

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 This embodiment discloses a kind of synthetic method of isocyanate curing agent, and described method step is as follows:

[0019] 1) Prepare a silicone-modified isocyanate with an NCO% (NCO% refers to the isocyanate group content in the polyisocyanate, ie the NCO content) of 8.6%.

[0020] Put aminopropyltriethoxysilane in a 250ml four-neck flask 110.5g, add diethyl maleate in a 250ml constant pressure dropper 86g, add diethyl maleate dropwise at room temperature, control the temperature below 45°C and add dropwise with nitrogen protection. After the dropwise addition, the temperature was raised to 70°C, and the material was kept for 48 hours to obtain a siloxane prepolymer with secondary amino groups.

[0021] (Reaction description: one molecule of aminopropyltriethoxysilane is added to one molecule of diethyl maleate to generate aspartic acid ester).

[0022] 2) Add 39.3g of the prepolymer to a 250ml constant pressure dropper, and add NCO%=21.7% h...

Embodiment 2

[0024] Embodiment 2 This embodiment discloses a kind of synthetic method of isocyanate curing agent, and described method step is as follows:

[0025] 1) Prepare a silicone-modified isocyanate with an NCO% (NCO% refers to the isocyanate group content in the polyisocyanate, ie the NCO content) of 12%.

[0026] Put 89.5g of aminopropyltrimethoxysilane into a 250ml four-neck flask, add 86g of diethyl maleate into a 250ml constant pressure dropper, add diethyl maleate dropwise at room temperature, and control the temperature at 50°C Add dropwise and protect with nitrogen. After the dropwise addition, the temperature was raised to 70° C., and the material was kept for 48 hours to obtain a siloxane prepolymer with secondary amino groups.

[0027] 2) Add 35.1g of the prepolymer to a 250ml constant pressure dropper, add 87.4g of hexamethylene diisocyanate trimer with NCO%=21.7% to a 250ml four-necked flask, and dropwise add prepolymer.

[0028] After dropping, the temperature was r...

Embodiment 3

[0029] Embodiment 3 This embodiment discloses a synthetic method of an isocyanate curing agent, and the steps of the method are as follows:

[0030] 1) Prepare a silicone-modified isocyanate with an NCO% (NCO% refers to the isocyanate group content in the polyisocyanate, ie the NCO content) of 8.5%.

[0031] Put 89.5g of aminopropyltrimethoxysilane into a 250ml four-neck flask, add 114g of dibutyl maleate into a 250ml constant pressure dropper, add dibutyl maleate dropwise at room temperature, and control the temperature at 50°C Add dropwise and protect with nitrogen.

[0032] After the dropwise addition, the temperature was raised to 70° C., and the material was kept for 48 hours to obtain a siloxane prepolymer with secondary amino groups.

[0033] 2) Add 101g of the prepolymer to a 250ml constant pressure dropper, add 145g of hexamethylene diisocyanate trimer with NCO%=21.7% to a 250ml four-necked flask, and add the prepolymer dropwise below 20°C body.

[0034] After drop...

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Abstract

The invention belongs to the field of chemical processing, and particularly relates to a synthesis method of an isocyanate curing agent. The synthesis method comprises the following steps: (1) synthesis of an organic silicon modified polyaspartate prepolymer: taking amino siloxane, dropwise adding maleate in equal molar weight with the amino siloxane, and carrying out heat preservation treatment after dropwise adding is completed, thus obtaining the polyaspartate prepolymer; (2) synthesis of the isocyanate curing agent: dropwise adding the polyaspartate prepolymer into an isocyanate tripolymer which is equivalently in equal molar weight with the polyaspartate prepolymer, and carrying out heat preservation after the dropwise adding is completed, thus obtaining the organic silicon modified isocyanate curing agent. In the technology, the rising of reaction temperature is not vigorous, the speed is controllable, and synthetic isocyanate is low in viscosity and can be directly applied to the industry of two-component polyurethane coating; silicon oxygen bonds and aspartate structures are introduced to polyurethane, so that the adhesion of a polyurethane coating film can be effectively increased, and the properties of high temperature resistance, aging resistance, salt fog resistance and the like are increased; the market prospect and the economic value are huge.

Description

technical field [0001] The invention belongs to the field of chemical processing, and in particular relates to a method for synthesizing an isocyanate curing agent. Background technique [0002] Polyurethane coating is a widely used protective coating, but it also has disadvantages such as low temperature resistance, poor adhesion, poor aging resistance, and poor salt spray resistance. [0003] Silane can react with many inorganic and organic materials and is a very multifunctional product. As a coupling agent, crosslinking agent and surface modifier, organosilane is widely used in many fields with its unique properties, from adhesives, to coatings to casting adhesives and more. [0004] As a coupling agent, organosilane can form covalent bonds with silanol groups on the surface of glass fibers or molecules on the surface of other inorganic fillers; in addition, siloxane coupling agents also contain a different functional group and polymerization Molecular bonding to obtai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/38C08G18/73C09D175/04
CPCC08G18/3893C08G18/73C09D5/18C09D175/04
Inventor 吕文章刘小卿罗善锴谢夏陆朱龙晖邱小勇邬茳
Owner SHENZHEN FEIYANG JUNYAN TECH DEV
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