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Process for preparation of meta-benzene dimethanamine by continuous hydrogenation reaction in stirring vessel

A technology for m-xylylenediamine and isophthalonitrile is applied in the field of continuous hydrogenation of isophthalonitrile stirred tank to prepare m-xylylenediamine, which can solve the problems of easy wear and tear of catalysts, broken and loss, complicated operation steps, and equipment utilization rate. Low problems, to achieve the effect of inhibiting the formation of by-products, high hydrogen utilization rate, and high equipment utilization rate

Active Publication Date: 2009-01-07
江苏德纳化学股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to provide a method for preparing m-xylylenediamine by continuous hydrogenation in a stirred tank, which can overcome the complicated operation steps, high labor intensity, easy wear and tear of the catalyst, and the equipment utilization rate. Low disadvantages, realize the continuous hydrogenation production of m-xylylenediamine in a stirred tank, and achieve the technical effects of high-efficiency hydrogenation, continuous catalyst regeneration, and recycling

Method used

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  • Process for preparation of meta-benzene dimethanamine by continuous hydrogenation reaction in stirring vessel
  • Process for preparation of meta-benzene dimethanamine by continuous hydrogenation reaction in stirring vessel
  • Process for preparation of meta-benzene dimethanamine by continuous hydrogenation reaction in stirring vessel

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Embodiment 1

[0026] Embodiment 1 adopts the method for continuous hydrogenation of the present invention to prepare m-xylylenediamine, and its technological process is as follows figure 1 shown.

[0027]The hydrogenation reactor is composed of three stirred tanks 2, 3 and 4 connected in series. In the hydrogenation reactor, the mixture of isophthalonitrile and solvent and hydrogen are contacted with the granular solid catalyst to carry out continuous hydrogenation reaction. The reaction material and catalyst composed of isophthalonitrile and solvent are sent into the first stirred tank reactor 2 through the conveying device 7, and then overflow from the upper part of the first stirred tank reactor 2 into the second stirred tank reactor 3 , and then overflows from the upper part of the second stirred tank reactor 3 into the third stirred tank reactor 4. The hydrogen enters the three stirred tank reactors 2, 3 and 4 respectively, and the unreacted hydrogen from the tops of the three stirred...

Embodiment 2～3

[0031] Examples 2 and 3 prepared m-xylylenediamine by continuous hydrogenation according to the process method of Example 1. The difference lies in the difference in hydrogenation reaction temperature and pressure.

[0032] The reaction results are shown in Table 1.

[0033] Table 1 Raney nickel catalyzed continuous hydrogenation of isophthalonitrile to prepare m-xylylenediamine reaction results

[0034]

Embodiment 4～6

[0036] Examples 4-6 According to the process method of Example 1, m-xylylenediamine was prepared by continuous hydrogenation, using an amorphous nickel catalyst.

[0037] According to the process method of Example 1, m-xylylenediamine was prepared by continuous hydrogenation. Reaction raw material composition: 20% (weight) of isophthalonitrile, 40% (weight) of methanol, 40% (weight) of toluene, use commercially available amorphous nickel catalyst, and its nickel content is 88.1% (weight). The feed rate of reaction raw materials is 180 kg / hour, the reaction temperature and pressure are shown in Table 2, the stirring speed is 200 rpm, the solid catalyst and liquid weight ratio in the reactor is 0.07: 1, the hydrogen circulation rate is 85 standard cubic meters / hour, and the material is in The total residence time in the reactor was 4 hours. Catalyst regeneration conditions: temperature 60°C, pressure 6.2MPa, solid catalyst to solvent weight ratio in regenerator 0.2:1, regenerat...

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Abstract

The invention discloses a method for preparing m-xylene diamine by continuous hydrogenation in a stirring kettle, which adopts m-phthalonitrile as the raw material and carries out multi-phase hydrogenation. The method is characterized in that the mixture of m-phthalonitrile and a solvent and hydrogen contact a granular solid catalyst in a hydrogenation reactor including at least two stirring kettles connected with each other in series to carry out continuous hydrogenation reaction; the reactive solution and the solid catalyst flowing from the end-stage stirring kettle are continuously fed into a separator for liquid-solid separation; the separated reactive solution is separated to obtain the final product; and the separated catalyst can be recycled after regeneration and returned to the hydrogenation reactor. Compared with the intermittent hydrogenation process, the method has the advantages of simple operation, high equipment utilization rate and hydrogenation efficiency, and continuous regeneration and cycle use of the catalyst, and can achieve automatic continuous production of m-xylene diamine.

Description

technical field [0001] The invention relates to a method for preparing m-xylylenediamine, in particular to a method for preparing m-xylylenediamine by continuous hydrogenation of isophthalonitrile in a stirred tank. Background technique [0002] m-Xylylenediamine (MXDA for short, CAS1477-55-0) is an aliphatic amine containing an aromatic ring, which is widely used because of its excellent physical and chemical properties. m-xylylenediamine is a low-toxic epoxy resin curing agent with excellent performance, excellent curing performance at room temperature, excellent heat resistance, water resistance and chemical corrosion resistance; it can be used to synthesize polyamide (MX nylon); it is also It can be used in the synthesis of polyurethane raw material m-xylene diisocyanate (XDI); it is also an important fine chemical raw material, which is effectively used in rubber crosslinking agents, stabilizers, plastic materials, fiber finishing agents, agricultural chemicals (drugs) ...

Claims

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Application Information

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IPC IPC(8): C07C211/27C07C209/48
CPCY02P20/584
Inventor 秦怡生秦旭东朱德宝段启伟陈荣福蒋大智
Owner 江苏德纳化学股份有限公司
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