Heat-sensitive tertiary amine catalyst, quaternized derivative, preparation and application thereof

A technology of tertiary amine catalysts and derivatives, which is applied in the field of new heat-sensitive tertiary amine catalysts and their quaternary ammonium salt derivatives, which can solve problems such as poor storage stability, troubles in the spraying industry, and short shelf life.

Active Publication Date: 2021-07-06
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In addition, dibutyltin dilaurate and stannous octoate are considered to be the strongest metal gel catalysts for polyols and isocyanates, but because they are easily hydrolyzed, the combin

Method used

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  • Heat-sensitive tertiary amine catalyst, quaternized derivative, preparation and application thereof
  • Heat-sensitive tertiary amine catalyst, quaternized derivative, preparation and application thereof
  • Heat-sensitive tertiary amine catalyst, quaternized derivative, preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0076] The preparation of embodiment 1 thermosensitive catalyst

[0077] One, the preparation of the thermosensitive catalyst shown in formula I structure:

[0078] 1) Preparation of the intermediate: Under the condition of 1MPa nitrogen protection, 300g of acetic acid and 946.5g of tetraethylenepentamine were reacted in a 5L reactor at 200°C for 1h under the action of 2000ml of tetrahydrofuran to obtain the intermediate, and the conversion rate reached 96%. Then water and tetrahydrofuran are azeotropically distilled until the water content is lower than 0.5%; after cooling, about 1120 g of tetraethylenepentamine imidazoline derivative intermediates are obtained;

[0079] 2) preparation of palladium series catalyst: 19.06g palladium sulfate and 3.12g ruthenium sulfate, 0.96g rhodium sulfate are dissolved in 70 ℃ of deionized waters and form the homogeneous solution of concentration about 30wt%; Then add 85.4g carrier diatomite, at 70 Rotate and impregnate at ℃ for 5.5 hours, ...

Embodiment 2

[0082] The preparation of embodiment 2 thermosensitive catalysts

[0083] 1) Preparation of intermediate: Using a synthesis process similar to that of Example 1, under 1MPa nitrogen protection conditions, 629g of propionic acid and 946.5g of tetraethylenepentamine were reacted in a 5L reactor at 200°C for 1h under the action of 2000ml of tetrahydrofuran The intermediate was obtained, the conversion rate reached 97%, and then the water and tetrahydrofuran were azeotropically distilled out until the water content was lower than 0.5%. After cooling, about 1295g of the imidazoline derivative intermediate of tetraethylenepentamine was obtained.

[0084] 2) Preparation of palladium series catalyst: 130.38g palladium nitrate and 1.255g ruthenium nitrate, 2.8g rhodium nitrate are dissolved in 80 DEG C of deionized water to form a homogeneous solution with a concentration of about 30wt%; then add 27.86g carrier alumina, and Rotate and impregnate at 80°C for 5.5 hours, then gradually ev...

Embodiment 3

[0087] The preparation of embodiment 3 thermosensitive catalysts

[0088] 1) Preparation of intermediates: using a synthesis process similar to Example 1, under 1MPa nitrogen protection conditions, 488.48g of benzoic acid and 946.5g of tetraethylenepentamine were reacted in a 5L reactor at 200°C under the action of 2000ml of tetrahydrofuran The intermediate was obtained in 1 hour, and the conversion rate reached 98%, and then water and tetrahydrofuran were azeotropically distilled until the water content was lower than 0.5%; after cooling, about 1411 g of an imidazoline derivative intermediate of tetraethylenepentamine was obtained.

[0089] 2) Preparation of palladium series catalyst: 65.19g palladium nitrate and 6.72g ruthenium nitrate, 0.14g rhodium nitrate are dissolved in 80 DEG C of deionized water to form a homogeneous solution with a concentration of about 30wt%; then add 61.94g carrier silicon dioxide, Rotate and impregnate at ℃ for 5.5 hours, then gradually evaporate...

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Abstract

The invention relates to a heat-sensitive tertiary amine catalyst, a quaternized derivative, preparation and application thereof, and belongs to the field of polymer synthesis. The structural formula of the heat-sensitive tertiary amine catalyst is shown as a formula I, wherein in the formula I, R1 is selected from substituted or unsubstituted C1-C10 alkyl, alkenyl, aryl or aralkyl, n is an integer, and n is more than or equal to 1 and less than or equal to 7. According to the invention, the obtained thermosensitive tertiary amine catalyst can efficiently catalyze foaming reaction of water and isocyanate at a temperature of 100 DEG C or below, wherein the catalytic effect of the thermosensitive tertiary amine catalyst is not weaker than that of BDMAEE and PMDETA; and the obtained thermosensitive tertiary amine catalyst can efficiently catalyze a gel reaction of polyol and isocyanate at a temperature of 100 DEG C or above, wherein the effect is not weaker than that of TEDA.

Description

technical field [0001] The invention relates to a novel heat-sensitive tertiary amine catalyst and a quaternary ammonium salt derivative thereof applied in the field of rigid polyurethane foam, and belongs to the field of polymer synthesis. Background technique [0002] Spraying rigid polyurethane foam is a type of open-celled or in-situ spraying process formed by chemical reactions in the presence of polyisocyanate and polyol liquid raw materials and additives such as surfactants, catalysts, crosslinking agents and blowing agents. Closed-cell foam products. Spray foam molding refers to a molding method in which the raw material of polyurethane rigid foam is directly sprayed onto the surface of the object and foamed on the surface. [0003] Commonly used catalysts in traditional spraying compositions include bis-(dimethylaminoethyl) ether (BDMAEE), pentamethyl-diethylenetriamine (PMDETA), triethylenediamine solution, dibutyltin dilaurate solution, Stannous octoate solution...

Claims

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Application Information

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IPC IPC(8): C08G18/20C08G18/18C08G18/48C08G18/42C08J9/14C07D233/24C08G101/00
CPCC08G18/2027C08G18/1875C08G18/4018C08G18/42C08G18/48C08J9/144C07D233/24C08G2101/00C08J2203/14Y02P20/584
Inventor 丁宗雷高杭滕向刘子厚刘赵兴尚永华孙晔
Owner WANHUA CHEM GRP CO LTD
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