Catalyst for synthesizing 1,3-cyclohexanedimethanamine through hydrogenation of m-xylylenediamine and preparation method thereof

A technology of m-xylylenediamine and cyclohexyldimethylamine, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, organic compound/hydride/coordination complex catalysts, etc., which can solve the problem of easy loss of active components, It is prone to side reactions, difficult to separate deamination inhibitors and products, etc., and achieves the effect of moderate acidity, tight combination, and weakened acidity

Active Publication Date: 2021-01-05
FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In view of the problems that the active components of existing catalysts are easy to lose, side reactions are easy to occur, and deamination inhibitors and products are difficult to separate, it is necessary to develop a m-benzene catalyst that is not easy to lose active components, has a long service life, high selectivity, and easy separation of products. Dimethylamine Hydrogenation Catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Preparation of SAPO-11 mesoporous molecular sieve with isomorphic replacement of Ru-Pr: The molar ratio of KH-560, pseudoboehmite, phosphoric acid, diisopropylamine and deionized water is 1:1.7:2:1.1: A scale of 40 weighs well. Add 11.7g pseudo-boehmite to a mixture of 23.1g phosphoric acid (concentration 85wt%), 11.1g diisopropylamine and 72.0g deionized water, add 1.9g hydrated ruthenium trichloride (ruthenium content 43wt%), 0.7 g Pr(NO 3 ) 3 , after stirring evenly, add 23.6g KH-560 respectively, stir fully at 25°C until a uniform gel is obtained, put the gel into a stainless steel autoclave and seal it, crystallize at a constant temperature of 120°C for 6 hours, and wait until the crystallization is complete, the product Centrifuge, wash with 80°C distilled water until the pH value remains constant, dry at 100°C, and calcinate in a muffle furnace at 400°C for 2 hours to obtain Ru-Pr isomorphously substituted SAPO-11.

[0049] (2) Organic amine modification: ...

Embodiment 2

[0052] (1) Preparation of SAPO-11 mesoporous molecular sieve with isomorphic substitution of Ru-Nd: The molar ratio of KH-560, pseudoboehmite, phosphoric acid, di-n-propylamine and deionized water is 1:1.8:1.9:1.2: A scale of 45 weighs well. Add 12.4g pseudoboehmite to a mixture of 21.9g phosphoric acid (concentration 85wt%), 12.1g di-n-propylamine and 81.0g deionized water, add 1.9g hydrated ruthenium trichloride (ruthenium content 43wt%), 0.5 g NdCl 3 , after stirring evenly, add 23.6g KH-560 respectively, stir fully at 25°C until a uniform gel is obtained, put the gel into a stainless steel autoclave and seal it, crystallize at a constant temperature of 130°C for 7 hours, and wait until the crystallization is complete, the product Centrifuge, wash with distilled water at 80°C until the pH value remains constant, dry at 100°C, and calcinate at 500°C in a muffle furnace for 1.5h to obtain Ru-Nd isomorphously substituted SAPO-11.

[0053] (2) Organic amine modification: The ...

Embodiment 3

[0056] (1) Preparation of SAPO-11 mesoporous molecular sieve with isomorphic replacement of Ru-Pr: The molar ratio of KH-590, pseudoboehmite, phosphoric acid, diisopropylamine and deionized water is 1:1.9:1.8:1.3: A scale of 50 weighs well. Add 15.4g pseudoboehmite to a mixture of 20.8g phosphoric acid (concentration 85wt%), 9.6g diethylamine and 90.0g deionized water, add 1.9g hydrated ruthenium trichloride (ruthenium content 43wt%), 0.5 g PrCl 3 , after stirring evenly, add 19.6g KH-590 respectively, stir fully at 25°C until a uniform gel is obtained, put the gel into a stainless steel autoclave and seal it, and crystallize at a constant temperature of 125°C for 8 hours. After the crystallization is complete, the product Centrifuge, wash with 80°C distilled water until the pH value remains unchanged, dry at 100°C, and calcinate in a muffle furnace at 450°C for 4 hours to obtain Ru-Pr isomorphously substituted SAPO-11.

[0057] (2) Organic amine modification: The molar rati...

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Abstract

The invention relates to the technical field of catalysts, in particular to a catalyst for synthesizing 1,3-cyclohexanedimethylamine through hydrogenation of m-xylylenediamine and a preparation methodof the catalyst. The catalyst for synthesizing 1,3-cyclohexanedimethanamine through hydrogenation of m-xylylenediamine comprises a carrier, an active component doped on the carrier and an accelerant,wherein the carrier of the catalyst is an SAPO-11 mesoporous molecular sieve, the active component is metal Ru, and the accelerant is one or more selected from the group consisting of Pr, Nd, Mo, Luand Tm. According to the catalyst for synthesizing 1,3-cyclohexanedimethanamine through hydrogenation of m-xylylenediamine, the active component is not easy to lose, the service life is long, and selectivity is high. The invention also provides the preparation method of the catalyst.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a catalyst for synthesizing 1,3-cyclohexanedimethylamine by hydrogenation of m-xylylenediamine and a preparation method thereof. Background technique [0002] 1,3-cyclohexanedimethylamine is an important chemical intermediate, which is widely used in the chemical industry. It is mainly used as a curing agent for epoxy resins. It has low volatility, is not easy to crystallize, fast curing speed, yellowing resistance, With the advantages of good weather resistance and good transparency, it is widely used in the fields of beauty joints, composite materials, epoxy floors and structural adhesives. Especially as a curing agent for beauty joints, it has an irreplaceable role. It can also be used to synthesize polyurethane with high refractive index and good transparency. [0003] The hydrogenation method of m-xylylenediamine (MXDA) is the main production method of 1,3-cyclohexyldime...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/85B01J31/02B01J37/03B01J37/02B01J37/16C07C209/72C07C211/18
CPCB01J29/85B01J31/0274B01J31/0275B01J37/0203B01J37/036B01J37/16B01J2229/183C07C209/72C07C2601/14C07C211/18
Inventor 岳林王敏黄森彪廖广明
Owner FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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