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

A technology of m-xylylenediamine and isophthalonitrile, which is applied in the field of preparation of m-xylylenediamine, can solve the problem of fast decline rate of catalytic activity of catalysts, easy wear and tear of catalysts, and inconvenience of disassembly, activation and regeneration and other problems, to achieve the effect of suppressing the formation of by-products, not easy to wear and tear, and high utilization rate of hydrogen

Active Publication Date: 2011-07-20
江苏德纳化学股份有限公司
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Problems solved by technology

[0005] In the above-mentioned method in the prior art, the preparation of m-xylylenediamine by the fixed-bed hydrogenation of isophthalonitrile has problems such as the rapid decline rate of the catalytic activity of the catalyst, the inconvenience of disassembly, activation and regeneration, and the traditional stirred tank batch method In the hydrogen process, each operation has to go through repeated frequent operation steps such as feeding, replacement, reaction, and discharging. Not only is the labor intensity high, the catalyst life is short, the catalyst is easy to wear, break and lose, and the utilization rate of the equipment is low, and the hydrogen gas is lost during the operation. Large amount, frequent switching operation of reaction equipment under high and low pressure conditions will increase the fatigue strength of the reactor, thereby reducing the life of the reactor, and it is difficult to realize automatic production

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

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Embodiment 1

[0027] Embodiment 1 adopts the method described in the present invention to prepare m-xylylenediamine by the continuous hydrogenation of isophthalonitrile, and its technological process is as follows figure 1 shown.

[0028] Hydrogen, reaction raw materials (isophthalonitrile and solvent) and catalyst enter the slurry bed reactor 2 from the lower part to carry out continuous hydrogenation reaction of isophthalonitrile, and the reaction materials realize gas-liquid separation in the head space of reactor 2. The tail gas discharged from the top of the reactor 2, that is, the unreacted hydrogen is recycled after being pressurized by the compressor 1; the liquid-solid mixture extracted from the top of the reactor 2 enters the liquid-solid separator 3 for liquid-solid separation, so that the solid catalyst and The reaction solution was separated. The separated solid catalyst enters the stirred tank regenerator 4, adds an appropriate amount of solvent, and is regenerated by washing...

Embodiment 2～5

[0032] Embodiments 2-5 Continuously prepare m-xylylenediamine according to the process method of embodiment 1. The difference lies in the catalyst used in the hydrogenation reaction and the reaction temperature and pressure. When using Raney nickel catalyst, Raney nickel is a commercially available Raney nickel catalyst, and its nickel content is 87.5% (weight); Raney nickel catalyst and liquid weight ratio 0.08: 1, 120 standard cubic meters / hour of hydrogen circulation , The residence time of the material in the reactor is 2.25 hours. The Raney nickel catalyst regeneration conditions were the same as in Example 1 except that the regeneration time was 3 hours.

[0033] The reaction results are shown in Table 1.

[0034] The reaction result of preparing m-xylylenediamine by continuous hydrogenation of isophthalonitrile in table 1

[0035]

Embodiment 6

[0037] Embodiment 6 adopts the method described in the present invention to prepare m-xylylenediamine by the continuous hydrogenation of isophthalonitrile, and the catalyst regeneration adopts a slurry bed regenerator, and its technological process is as follows figure 2 shown.

[0038] Hydrogen, reaction raw materials (isophthalonitrile and solvent) and catalyst enter the slurry bed reactor 2 from the lower part to carry out continuous hydrogenation reaction of isophthalonitrile, and the reaction materials realize gas-liquid separation in the head space of reactor 2. The tail gas discharged from the top of the reactor 2, that is, the unreacted hydrogen is recycled after being pressurized by the compressor 1; the liquid-solid mixture extracted from the upper part of the reactor 2 enters the liquid-solid separator 3 to separate the catalyst and the reaction liquid. Add an appropriate amount of solvent to the separated catalyst, enter the slurry bed regenerator 4, wash and rege...

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Abstract

The invention discloses a method for preparing m-xylene diamine by continuous hydrogenation, 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 slurry bed reactor to carry out continuous hydrogenation reaction; the reactivesolution and the solid catalyst are continuously fed into a separator for liquid-solid separation; the separated reactive solution is separated to obtain the final product; and the separated catalystcan be recycled after regeneration and returned to the slurry bed reactor. The method can achieve continuous hydrogenation of m-phthalonitrile, and has the advantages of good conversion rate and selectivity, convenient operation, and high equipment utilization rate and hydrogenation efficiency, and the catalyst is not easy to abrade and crush and can be continuously regenerated and recycled.

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. 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) and Surfactants a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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