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Preparation method of 4,4'-aminodiphenylamine

The technology of diaminodiphenyl ether and dinitrodiphenyl ether is applied in the field of fine chemical industry, which can solve the problems of complex product purification conditions, large environmental pollution and high production cost, and achieves improved appearance quality, less environmental pollution and product quality. Good results

Inactive Publication Date: 2009-02-04
SHANGHAI HUAYI ENERGY CHEM
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  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by this invention is to provide a kind of preparation method of 4,4'-diaminodiphenyl ether, to overcome the energy consumption of existing preparation method and the high production cost that the amount of Pd in ​​solvent raw material, catalyst causes, the environment Defects of unstable quality and low yield caused by heavy pollution and complicated product purification conditions

Method used

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  • Preparation method of 4,4'-aminodiphenylamine
  • Preparation method of 4,4'-aminodiphenylamine

Examples

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Embodiment 1

[0025] Put 18Kg of 4,4'-dinitrodiphenyl ether, 90g of Pd / c catalyst with a Pd content of 1%, and 36Kg of methanol solvent into a 100L hydrogenation reactor with a stirring device. The reactor is first replaced with nitrogen three times, and then hydrogen Replace three times, feed steam into the reactor jacket to heat up the temperature, control the reaction temperature at 70°C and the reaction pressure at 0.4MPa to carry out the catalytic hydrogenation reduction reaction. After the reaction is finished, the reaction solution is filtered and put into a crystallization tank equipped with a stirring device for cooling and crystallization. When the temperature of the tank is cooled below 40°C, the crystallization is complete, and 4,4'-diaminodiphenyl ether crystallizes out. The material is first filtered to remove the solvent, and the solvent is recycled after recycling. The solid 4,4'-diaminodiphenyl ether is washed twice with methanol solvent, and the product is dried to obtain 4...

Embodiment 2

[0027] In the 100L hydrogenation reactor with agitator, drop into 10Kg4, 4'-dinitrodiphenyl ether, 100gPd content is the Pd / c catalyst of 1%, 60Kg ethylene glycol solvent, and the reactor is replaced with nitrogen three times earlier, and then Replace with hydrogen three times, feed steam into the reactor jacket to heat up, control the reaction temperature at 95°C and the reaction pressure at 3.0MPa to carry out the catalytic hydrogenation reduction reaction. After the reaction is finished, the reaction solution is filtered and put into a crystallization tank equipped with a stirring device for cooling and crystallization. When the temperature of the tank is cooled below 40°C, the crystallization is complete, and 4,4'-diaminodiphenyl ether crystallizes out. The material is first filtered to remove the solvent, and the solvent is recycled after recycling. The solid 4,4'-diaminodiphenyl ether is washed with methanol solvent for 3 times, and the product is dried to obtain 4,4'-dia...

Embodiment 3

[0029] Other conditions are the same as in Example 1, except that the catalyst adopts a Pd / c catalyst with a content of 2.9%. 12.62 kg of 4,4'-diaminodiphenyl ether polymer grade product was obtained, which appeared as white granular crystals, with a melting point of 190.8-191.2° C., a purity of 99.8% (HPLC), and a molar yield of 91.1%.

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Abstract

The invention relates to a preparation method of 4, 4'-diamino diphenyl ether and belongs to the technical field of fine chemical industry. The reaction includes the following steps: the catalytic hydrogenation reduction reaction of the 4, 4'-diamino diphenyl ether is carried out in Pd / c catalyst and alcoholic solvents under the temperature of 70 to 95 DEG C, and the 4, 4'-diamino diphenyl ether product is obtained by the separation, crystallization, solvent washing and drying of the chemical product by the catalyst; the Pd content in the Pd / c catalyst is 0.5 to 3 percent. The method is characterized by low reaction temperature, short process route, high yield ratio, low cost of solvents and catalyst, good product quality and low environmental pollution and is suitable for the industrial preparation of the 4, 4'-diamino diphenyl ether.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a preparation method of 4,4'-diaminodiphenyl ether. Background technique [0002] 4,4'-Diaminodiphenyl ether is a high value-added fine chemical organic product. It is one of the important raw materials of new special engineering plastics such as polyimide, polyetherimide, polyesterimide, polyamideimide, polymaleimide, polyarimide and other high temperature resistant resins. It is also the raw material for the synthesis of 3,3',4,4'-tetraaminodiphenyl ether, which is used to prepare a series of new heat-resistant aromatic heterocyclic polymer materials such as polybenzimidazole, polyphenylquinoline, polyimidazole An important monomer of pyridine. It can also be used as a raw material and crosslinking agent for synthetic polymer materials such as high-performance heat-resistant epoxy resin and polyurethane. At the same time, it can also be used to replace the carcinogenic benzidin...

Claims

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Application Information

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IPC IPC(8): C07C217/90C07C213/02
Inventor 金生亚谢振华季维鹏
Owner SHANGHAI HUAYI ENERGY CHEM
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