Method for producing H12MDA through hydrogenation reaction

A hydrogenation reaction, MDA technology, applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of difficult product separation and reuse of sol catalysts, and achieve easy regeneration, high activity and durability. Effect

Active Publication Date: 2007-10-10
WANHUA CHEMICAL (NINGBO) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The polymer-protected noble metal sol is loaded on the inorganic carrier to realize the immobilization of the metal sol catalyst, which not only solves the problem that the sol catalyst is not ...

Method used

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  • Method for producing H12MDA through hydrogenation reaction
  • Method for producing H12MDA through hydrogenation reaction
  • Method for producing H12MDA through hydrogenation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Preparation of catalyst 1

[0058] 0.1g Ru(NO 3 ) 3 Dissolve in 50mL of water, add 3.9mL of 5g / L Tween20 (manufactured by DuPont) solution to Ru(NO 3 ) 3 In the aqueous solution, stir for 1h, add 4.5g / L NaBH dropwise 4 Aqueous solution of 40mL, after the reduction is completed, a metal ruthenium colloid protected by Tween20 is obtained. Then add 2 g of activated carbon, stir for 2 hours, filter and wash with water to prepare a 3% Ru / C catalyst. The average particle size of the metallic ruthenium colloidal particles measured by the HRTEM method (dispersed in ethanol, measured by copper mesh) is 3 nm. The loading rate of ruthenium metal on the carrier reaches 99.8%.

Embodiment 2

[0060] Preparation of catalyst 2

[0061] 0.1gRuCl 3 3H 2 O is dissolved in 50mL water, and 5mL of 5g / L Span20 (manufactured by DuPont) solution is added to RuCl 3 In the aqueous solution, stir for 1h, add 4.5g / L NaBH dropwise 4 Aqueous solution of 40mL, after the reduction is completed, a metal ruthenium colloid protected by Span20 is obtained. Then add 2 g of activated carbon, stir for 2 hours, filter and wash with water to prepare a 3% Ru / C catalyst. The average particle size of the metallic ruthenium colloidal particles measured by the HRTEM method (dispersed in ethanol, measured by copper mesh) is 3.2 nm. The loading rate of metal ruthenium on the carrier reaches 100%.

Embodiment 3

[0063] Preparation of catalyst 3

[0064] 0.2589g of ruthenium acetate was added to 400mL water with 0.2732g Span20 and 0.1943g Tween20 dissolved. Add 0.1374g NaBH dropwise under vigorous stirring 4 After the reduction is completed, the metal ruthenium colloid protected by Span20 and Tween20 is obtained. 2 g of activated carbon was added to the colloidal solution, stirred for 1.5 hours, filtered and washed with water, and rinsed with THF to prepare a 5% Ru / C catalyst. The average particle size of the metallic ruthenium colloidal particles measured by the HRTEM method (dispersed in ethanol, copper mesh) is 2.8 nm. The loading rate of metal ruthenium on the carrier reaches 100%.

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Abstract

This invention discloses a method for preparing 4, 4'-diamino dicyclohexylmethane (H12MDA) from 4, 4'-diamino diphenylmethane (MDA) via hydrogenation catalyzed by supported nanoscale Ru catalyst. The method comprises: performing stereoselective hydrogenation on MDA at 100-180 deg.C and 4-10 MPa in an intermittent autoclave for 1-9 h to obtain H12MDA. The MDA conversion rate is near 100%, the H12MDA weight yield is near 100%, and the trans-H12MDA content is below 25%. After the supported nanoscale Ru catalyst is continuously reused for above 30 times without supplementation, the MDA conversion rate is still near 100%, and the trans-H12MDA content is below 27%.

Description

Technical field [0001] The present invention relates to a method for preparing 4,4'-diaminodicyclohexylmethane (H 12 MDA) method, the hydrogenation reaction uses a supported nano ruthenium catalyst. Background technique [0002] 4,4’-Diaminodicyclohexylmethane (H 12 MDA) is an important raw material for the preparation of a new generation of anti-aging polyurethane "dicyclohexylmethane diisocyanate (HMDI)" with superior performance. It usually uses 4,4'-diaminodiphenylmethane (MDA) as the raw material. Under the action, H is obtained by high-temperature and high-pressure hydrogenation 12 MDA, then H 12 MDA is then phosgenated to obtain HMDI. This type of isocyanate has the characteristics of stable performance and strong oxidation resistance. It is widely used in the preparation of lightweight polyurethane coatings, paints, foam plastics, various elastomers, adhesives, fibers, synthetic leather and paving materials, etc. The application fields involve electromechanical, Ships, av...

Claims

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Application Information

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IPC IPC(8): C07C211/36C07C209/72
Inventor 吕连海马德强齐旺顺杜文强荣泽明罗务习胡爽郭方王越华卫琦丁建生
Owner WANHUA CHEMICAL (NINGBO) CO LTD
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