Use of n,n-dimethylcyclohexane tertiary amine derivatives as catalysts for preparing polyurethane and/or polyisocyanurate foams

A technology of dimethylcyclohexane tertiary amine and polyisocyanurate, which is applied in the field of preparation of gel-type catalyst N,N-dimethylcyclohexane tertiary amine derivatives, and can solve problems such as poor stability , to achieve the effect of stable system, good gel effect and low odor

Active Publication Date: 2022-01-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Therefore, in view of the mismatch between the existing amine catalysts and trans-1-chloro-3,3,3-trifluoropropene (HCFO-1233zd(E)), it is necessary to seek a new catalyst system to overcome the reaction Formula-1-Chloro-3,3,3-trifluoropropene (HCFO-1233zd(E)) combined with the defect of poor stability of polyether system

Method used

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  • Use of n,n-dimethylcyclohexane tertiary amine derivatives as catalysts for preparing polyurethane and/or polyisocyanurate foams
  • Use of n,n-dimethylcyclohexane tertiary amine derivatives as catalysts for preparing polyurethane and/or polyisocyanurate foams
  • Use of n,n-dimethylcyclohexane tertiary amine derivatives as catalysts for preparing polyurethane and/or polyisocyanurate foams

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Preparation of palladium series catalyst 1:

[0059] Dissolve 25.04g of palladium nitrate dihydrate, 0.14g of rhodium nitrate, and 2.76g of ruthenium acetate in 100ml of deionized water, heat to 60°C to form a homogeneous solution, then add 88.95g of alumina (average particle size 50μm, specific surface area 180m 2 / g, pore volume 0.30cc / g), in a water bath at 70°C for 5 hours and then gradually evaporated to dryness, then baked in an oven at 100°C for 16 hours; finally moved to a muffle furnace, in an air atmosphere at 3°C / The temperature was raised to 550°C for 8 hours, and the catalyst was obtained after natural cooling. The composition of the catalyst is as follows: Pd is 10wt%, Rh is 0.05wt%, Ru is 1wt%, and the rest is alumina. Based on the corresponding metal elements accounting for the total mass of the catalyst, the metal exists in an oxidized state and needs to be reduced during use.

Embodiment 2

[0061] Preparation of Palladium Series Catalyst 2:

[0062] Dissolve 5.01g of palladium nitrate dihydrate, 1.40g of rhodium nitrate, and 5.51g of ruthenium acetate in 100ml of deionized water, heat to 70°C to form a homogeneous solution, then add 95.5g of silicon dioxide (average particle size 60μm, specific surface area 240m 2 / g, pore volume 0.38cc / g), in a water bath at 60°C for 6 hours and then gradually evaporated to dryness, then baked in an oven at 120°C for 12 hours; finally moved to a muffle furnace, in an air atmosphere at 2°C / The temperature was raised to 600°C for 6 hours, and the catalyst was obtained after natural cooling. The composition of the catalyst is: Pd is 2wt%, Rh is 0.5wt%, Ru is 2wt%, and the rest is silicon dioxide. Based on the corresponding metal elements accounting for the total mass of the catalyst, the metal exists in an oxidized state and needs to be reduced during use.

Embodiment 3

[0064] Preparation of trans N,N,N,N-tetramethyl-1,4-cyclohexanediamine:

[0065] Add 4g of the palladium-based catalyst in Example 1 to a 1L reaction kettle, add methanol solvent as a primer, seal the reaction kettle, replace with nitrogen and hydrogen for three times, and activate the catalyst at a temperature of 240°C and a hydrogen pressure of 5MPa 6 hours. After that, the temperature was lowered, the pressure was released, and nitrogen was replaced three times, and the solvent was filtered out from the reaction kettle. Then add 100g of trans-1,4-cyclohexanediamine, replace with nitrogen and hydrogen three times in sequence, the initial hydrogen pressure is 2MPa, start stirring at 700 rpm, wait for the reaction temperature to rise to 160°C, and put the hydrogen Adjust the pressure to 3MPa and continue to flow hydrogen, start to flow 170g of 37% formaldehyde solution into the reactor at a speed of 2g / min with a convection pump, wait until the instantaneous flow rate of the ...

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Abstract

The invention provides a preparation method and application of N,N-dimethylcyclohexylamine derivatives. The method prepares cyclohexane tertiary amine derivatives through methylation of primary amine derivatives of cyclohexane, formaldehyde and hydrogen under the action of a catalyst at a certain temperature and pressure. The derivative of the cyclohexane tertiary amine of gained can be used as polyurethane / polyisocyanurate catalyst after purification, and the present invention is applicable to trans-1-chloro-3,3,3-trifluoropropene (HCFO-1233zd (E)) The blowing agent system can replace the tertiary amine catalyst with high activity and low steric hindrance as a use, and effectively avoid the tertiary amine catalyst with high activity and low steric hindrance from causing trans-1-chloro-3,3,3- Risk of decomposition of trifluoropropene (HCFO‑1233zd(E)).

Description

technical field [0001] The invention relates to a polyurethane and / or polyisocyanurate foam catalyst, especially suitable for a trans-1-chloro-3,3,3-trifluoropropene (HCFO-1233zd(E)) foaming system A preparation method and application of a new gel-type catalyst N,N-dimethylcyclohexane tertiary amine derivative. Background technique [0002] In recent years, the replacement of low boiling point compound blowing agents has become a hot spot in the field of polyurethane foam. At present, it has experienced the changes of four generations of blowing agents. Among them, the first generation blowing agent is represented by CFC-11, which has been widely used for decades due to its stable chemical properties, low toxicity, moderate boiling point, high foaming efficiency, and small thermal conductivity. It is the culprit that destroys the earth's ozone layer. After CFCs enter the stratosphere, they are exposed to strong ultraviolet radiation and release chlorine atoms, which are c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/18C08G18/22C08G18/24C08G18/40C08G18/42C08G18/48C08J9/14C08L75/08C08L75/04C08G101/00
CPCC08G18/1816C08G18/4804C08G18/14C08J9/149C08G18/4018C08G18/42C08G18/48C08G18/165C08G18/242C08G18/225C08J9/144C08J2375/08C08J2375/04C08J2203/162C08J2203/14C08G2101/00
Inventor 丁宗雷高杭刘振国陈杰孙晔杨洗滕向刘赵兴
Owner WANHUA CHEM GRP CO LTD
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