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M-xylylenediamine hydrogenation catalyst, preparation method and application thereof

A m-xylylenediamine and catalyst technology, which is applied in the field of hydrogenation catalyst and its preparation, can solve the problems of environmental pollution, large amount of catalyst, and affecting production efficiency, etc., to improve selectivity and stability, stabilize activity and selectivity , Improve the effect of adsorption and activation ability

Active Publication Date: 2020-06-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention uses liquid ammonia or small molecular organic amines as reaction solvents to carry out hydrogenation at low substrate concentration and mass space velocity, which also has the problems of low production efficiency and high energy consumption.
[0007] In summary, the main problems in the prior art are: (1) m-xylylenediamine mass space velocity is low, resulting in large catalyst consumption and high investment costs
In addition, under the condition of batch process, the large amount of catalyst may bring problems such as long filtration time of the reaction mother liquor, which affects the production efficiency; Consumption is high, increased production cost; (3) reaction condition is harsher, in order to obtain high 1,3-cyclohexanedimethylamine yield, generally adopt liquid ammonia or other small molecule organic amine etc. as reaction solvent, or utilize inorganic The catalyst is modified by alkali, and the hydrogenation reaction is carried out under high temperature and high pressure. The safety risk is high, and material leakage is prone to occur, causing environmental pollution.

Method used

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  • M-xylylenediamine hydrogenation catalyst, preparation method and application thereof
  • M-xylylenediamine hydrogenation catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Weigh 20g Ca(NO 3 ) 2 .4H 2 O, add 200g water to dissolve, then add 150g SBA-15 molecular sieve, heat up to 50°C, add 5g NaOH, stir for 5h, filter, wash with distilled water until the pH is 7, dry the filter cake at 100°C for 10h, and then dry it at 400°C Roast for 6h, cool down to room temperature, and set aside;

[0056] (2) Weigh the modified molecular sieve obtained in 100g step (1), 0.005g metal Eu, 0.05g Yb, join in 1L autoclave, fill 1MPa nitrogen replacement, repeat 3 times, add 200g liquid ammonia again, water bath is heated to Stir at 40°C for 5 hours, then cool down to room temperature, exhaust the nitrogen and liquid ammonia in the kettle, open the kettle, wash out the catalyst in the kettle with ethanol, filter out the carrier, wash with ethanol and distilled water respectively, and dry at 110°C; Place the dried carrier in a muffle furnace, bake it at 500°C for 5h under a nitrogen atmosphere, and then cool it down to room temperature for use;

[005...

Embodiment 2

[0060] Catalyst sample C2 was prepared by the same method steps as in Example 1, except that PEG-600 was not added in step (3), but 40 g of CTAB was added.

Embodiment 3

[0062] Catalyst sample C3 is prepared by the same method steps as in Example 1, and the difference is: in step (1), use 15gMg(NO 3 ) 2 .6H 2 O instead of 20g Ca(NO 3 ) 2 .4H 2 O, replace SBA-15 with 100gβ molecular sieve, RuCl in step (3) 3 .3H 2 O mass is 5.10g, H[AuCl 4 ] quality is 0.11g, the NaBH that is 1mol / L is added dropwise with the rate of 50mL / min 4 Aqueous solution 200mL, do not pass methylamine in the step (4), but pass into 4000g ethylenediamine with the speed of 1000g / h.

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Abstract

The invention provides a catalyst for synthesizing 1, 3-cyclohexanedimethylamine by hydrogenation of m-xylylenediamine and a preparation method thereof. The catalyst is composed of a carrier, and an active component and an auxiliary agent which are attached to the carrier; wherein the active component is composed of one or more of metals Rh, Pt, Pd, Ir, Au, Ag, Ni and Re and noble metal Ru; the auxiliary agent is composed of an auxiliary agent I and an auxiliary agent II, the auxiliary agent I is composed of metals Eu and Yb, the auxiliary agent II is selected from one or more of metals Li, Na, k, Cu, Co, Fe, Zn, Mn, La and Ce, and the carrier is a metal compound modified molecular sieve. Compared with the prior art, the catalyst can acquire a high raw material conversion rate and 1, 3-cyclohexanedimethylamine selectivity under low reaction temperature and pressure and high substrate concentration and reaction space velocity, is stable in performance and long in service life, can obviously improve the production efficiency and reduce the production cost, and is beneficial to industrial application.

Description

technical field [0001] The invention relates to a hydrogenation catalyst and a preparation method thereof, in particular to a catalyst for synthesizing 1,3-cyclohexanedimethylamine by hydrogenation of m-xylylenediamine and a preparation method thereof, belonging to the technical field of hydrogenation catalysts. Background technique [0002] m-Xylylenediamine can be used as an epoxy curing agent, but its freezing point is relatively high (14.1°C), which limits its application in low temperature environments, especially in cold winters. It is hydrogenated into 1,3-cyclohexanedimethylamine, the freezing point (<-25°C) is greatly reduced, and it has the advantages of high low-temperature curing activity and low toxicity. It is widely used in the fields of beauty joints, automotive composite materials, etc. . [0003] The prior art of m-xylylenediamine hydrogenation to synthesize 1,3-cyclohexanedimethylamine is mainly reported as follows: [0004] Patent CN 102690203 A, usi...

Claims

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Application Information

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IPC IPC(8): B01J29/04B01J29/48C07C209/72C07C211/18
CPCB01J29/045B01J29/48C07C209/72C07C211/18
Inventor 龚亚军张聪颖李海龙杨在刚郭爱国丁儒王静丁皓
Owner WANHUA CHEM GRP CO LTD
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