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Catalyst for synthesis of bis(aminomethyl)cyclohexane and preparation method and application thereof

A technology of diaminomethylcyclohexane and catalyst is applied in the field of catalytic hydrogenation, which can solve the problems of affecting production stability, increasing equipment investment, leakage of liquid ammonia, etc., so as to improve reaction activity and selectivity, and stabilize activity and selection. The effect of inhibition of sexual and deamination side reactions

Active Publication Date: 2019-11-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of volatile liquid ammonia or small molecule organic amines is likely to pollute the production environment, affect occupational health, and there are safety hazards such as liquid ammonia leakage. The recovery of liquid ammonia after the reaction is also a problem, which greatly increases equipment investment; adding alkali Metal hydroxide, due to the problem of alkali loss during the reaction process, needs to be supplemented in the subsequent catalyst application. It is difficult to accurately control the amount of addition, and it is difficult to maintain the stable activity and selectivity of the catalyst, thus affecting the stability of production.
On the other hand, the addition of a large amount of alkali metal hydroxide will cause equipment corrosion problems

Method used

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  • Catalyst for synthesis of bis(aminomethyl)cyclohexane and preparation method and application thereof
  • Catalyst for synthesis of bis(aminomethyl)cyclohexane and preparation method and application thereof
  • Catalyst for synthesis of bis(aminomethyl)cyclohexane and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Weigh 100g Mg(NO 3 ) 2 .6H 2 O, 500g distilled water, add to the beaker, stir to dissolve, then add 180gAl 2 o 3 , stirred at room temperature for 2h, then added dropwise 160g of 20% NaOH aqueous solution at a rate of 3g / min, continued to stir for 1h, filtered, washed with distilled water until neutral, and dried in a 110°C oven to obtain a filter cake After one night, it was calcined in a muffle furnace at 600° C. for 5 hours, and cooled to room temperature to obtain a magnesium-aluminum double metal oxide carrier, which was ready for use.

[0046] (2) Take by weighing the magnesium-aluminum double metal oxide carrier that 100g step (1) makes, 0.5g LiNO 3 (69), put it into a 500mL autoclave, and add 200g of distilled water to mix evenly, put on the kettle, heat to 120°C, and keep at this temperature for 4h. Lower the temperature, open the kettle, filter, wash, and dry the filter cake in an oven at 110°C overnight for use.

[0047] (3) Weigh 6.46g RuCl 3 .3H ...

Embodiment 2

[0050] Catalyst sample C2 was prepared by the same method steps as in Example 1, except that LiNO was not used in step (2). 3 , while using 2.18g Mn(NO 3 ) 2 .4H 2 O)(251) instead.

Embodiment 3

[0052] Catalyst sample C3 is prepared by the same method steps as in Example 1, except that Fe(NO 3 ) 3 .9H 2 O, while using 9.36g Cu(NO 3 ) 2 .3H 2 O(242) instead; NaBH in step (4) 4 The mass is 25.47g, dissolved in 500g distilled water.

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PUM

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Abstract

The invention relates to a catalyst for synthesis of bis(aminomethyl)cyclohexane. The catalyst is prepared from a carrier, active components and additives, wherein the active components and the additives adhere to the carrier. The active components are selected from one or more of metals such as Ru, Rh, Ni, Co, Pt and Pd, and preferably, the active components are the metal Ru and are selected fromone or more of the metals such as Rh, Ni, Co, Pt and Pd; and the additives comprise a first additive and a second additive, the first additive is selected from one or more of Mn, Cr, Li and Ca, and the second additive is selected from one or more of Fe, Cu, Zn, Ag, Sn, La and Ce. Compared with the prior art, the catalyst is high in activity, good in selectivity and long in life, liquid ammonia oralkali metal hydroxides do not need to be added in a reaction system to serve as an deamination inhibitor, and thus the hydrogenation of benzene dimethylamine can be catalyzed so as to obtain bis(aminomethyl)cyclohexane in high-activity and high-selectivity modes.

Description

technical field [0001] The invention relates to a hydrogenation catalyst and a preparation method thereof, in particular to a catalyst for synthesizing diaminomethylcyclohexane, a preparation method thereof and a hydrogenation reaction using the catalyst, belonging to the technical field of catalytic hydrogenation. Background technique [0002] Diaminomethylcyclohexane mainly includes 1,3-diaminomethylcyclohexane and 1,4-diaminomethylcyclohexane, which is an important fine chemical intermediate and is mainly used as a curing agent for epoxy resin. Its downstream can also be used to synthesize polyamide, polyurethane and so on. As an epoxy curing agent, it has the advantages of fast curing speed, good toughness and excellent yellowing resistance; its synthesized polyamide resin has high heat resistance and has special applications in fiber and film materials; its synthesized polyurethane It can be used in the manufacture of various light-resistant polyurethane coatings, elas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/63C07C211/18C07C209/72
CPCB01J23/8946B01J23/8986B01J23/63B01J23/8953C07C209/72C07C211/18
Inventor 龚亚军张聪颖杨在刚唐磊任树杰李鑫刘振国丁皓
Owner WANHUA CHEM GRP CO LTD
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