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Catalyst for preparing meta-xylylenediamine and application of catalyst

The technology of m-xylylenediamine and catalyst is applied in the field of synthesis of m-xylylenediamine and hydrogenation catalyst, which can solve the problems of complex separation, low activity and selectivity, and high composition, so as to optimize reaction process conditions and reduce Side reactions, the effect of improving selectivity

Active Publication Date: 2019-08-23
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to solve the catalyst existing in the prior art under the condition of continuous hydrogenation in a fixed bed due to problems such as polymerization and deamination, resulting in low activity and selectivity, and most of the solvents used in the current catalytic reaction are A variety of mixed solvents not only have high composition, but also complicated subsequent separation. In addition, the technical problem solved by the present invention is the use of the corresponding catalyst of the present invention

Method used

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  • Catalyst for preparing meta-xylylenediamine and application of catalyst
  • Catalyst for preparing meta-xylylenediamine and application of catalyst
  • Catalyst for preparing meta-xylylenediamine and application of catalyst

Examples

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Embodiment 1

[0022] Weigh 1000g of aluminum nitrate nonahydrate and deionized water to prepare 1L solution, pour it into a 3L glass reaction kettle with stirring and heating and raise the temperature to 60°C, add 18% ammonia solution dropwise, and carry out neutralization and precipitation. The neutralization time is 15 Minutes, adjust the final pH value to 7.6, age for 40 minutes, fix the crystal form, and obtain a filter cake after filtration; the filter cake is dried, pulverized and added with 5.2 g of forming aids magnesium stearate and 1.4 g of pore-forming aids carboxymethyl cellulose g, pressed into The tablets were then calcined at a temperature of 800° C. for 2 hours to obtain the carrier Z1. The physical and chemical data of the carrier are shown in Table 1.

Embodiment 2

[0024] Weigh 800g of aluminum nitrate and 200g of magnesium nitrate hexahydrate plus deionized water to prepare 1L of solution, pour it into a 3L glass reactor with stirring and heating and raise the temperature to 80°C, add 15% ammonia solution dropwise for neutralization and precipitation. The mixing time is 25 minutes, adjust the end point pH value to 7.2, age for 20 minutes, fix the crystal form, and obtain a filter cake after filtration; the filter cake is dried, pulverized and added with 1.9 g of forming aids magnesium stearate and pore-forming aids Sinensis Powder 3.0g, pressed into The tablets were then calcined at a temperature of 700° C. for 4 hours to obtain the carrier Z2. The physical and chemical data of the carrier are shown in Table 1.

Embodiment 3

[0026] Weigh 700g of aluminum nitrate and 350g of magnesium acetate tetrahydrate plus deionized water to prepare 1L of solution, pour it into a 3L glass reaction kettle with stirring and heating and raise the temperature to 70°C, add 10% ammonia solution dropwise for neutralization and precipitation. The mixing time is 35 minutes, adjust the end point pH value to 7.8, age for 30 minutes, fix the crystal form, and obtain a filter cake after filtration; the filter cake is dried, pulverized and added with 2.0 g of forming aid stearic acid, pore-forming aid carboxymethyl Cellulose 3.0g, pressed into The tablets were then calcined at a temperature of 900° C. for 2 hours to obtain the carrier Z3. The physical and chemical data of the carrier are shown in Table 1.

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Abstract

The invention discloses a catalyst for preparing meta-xylylenediamine and application of the catalyst, and belongs to the field of hydrogenation catalysts. Alumina or a mixture of magnesium and aluminum is adopted as a carrier, the active element is Ni, and the auxiliary agent 1 is one of Co and Mn; and the auxiliary agent 2 is one of Na and K, and preparation of the catalyst comprises the steps of preparation of the catalyst carrier, impregnation of the active component, impregnation of the auxiliary agents and activation of the catalyst. A preparation method has a simple process and low cost, and is suitable for industrial production, and the catalyst has suitable pores; through addition of the suitable additives, the reaction process conditions are optimized, and the catalyst has the characteristics of high activity, no easy clogging of the pores, a long service life and the like; and when the catalyst is applied to preparation of meta-xylylenediamine through hydrogenation of isophthalonitrile, the conversion rate of isophthalonitrile is 100%, and the selectivity to meta-xylylenediamine is 99% or above.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of m-xylylenediamine and a used hydrogenation catalyst. Background technique [0002] m-xylylenediamine, a colorless liquid at room temperature, is an important chemical raw material, used as a normal temperature, low-toxicity curing agent for epoxy resin, and also used as a raw material for photosensitive plastics, rubber additives, polyurethane resin and coatings and organic synthesis intermediates. [0003] In the prior art, the production process of catalytic hydrogenation of isophthalonitrile (IPN) is mainly used to prepare m-xylylenediamine, and the catalyst used is generally Raney nickel or Raney cobalt catalyst. Stirred tanks are often used for intermittent production. For example, JP54-41804 discloses a preparation method of m-xylylenediamine. The method uses Raney nickel or Raney cobalt catalysts, and uses a mixed solvent of low-carbon al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10B01J23/889B01J23/78B01J35/10B01J37/03B01J37/02B01J37/08C07C209/48C07C211/27
CPCC07C209/48B01J21/10B01J23/8892B01J23/78B01J37/0018B01J37/031B01J37/0201B01J35/613B01J35/615B01J35/635B01J35/633B01J35/647C07C211/27
Inventor 何明阳钱俊峰孙中华孙富安吴中陈群
Owner CHANGZHOU UNIV
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