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Method for preparing hexamethylene diamine by direct hydrogenation of adiponitrile under alkali-free conditions

A technology of adiponitrile and hexamethylene diamine, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of corrosion, environmental pollution, poor mechanical properties, etc.

Inactive Publication Date: 2018-05-29
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the Raney Ni-type catalyst used in the catalytic hydrogenation of adiponitrile has poor mechanical properties, is easily broken, and is difficult to separate from the product; has poor thermal stability, is prone to spontaneous combustion in the air, and is not easy to store; a large amount of lye is discharged during the preparation process, polluting the environment; the reaction process It is necessary to add alkali or ammonia water to inhibit the production of secondary and tertiary amines to improve the selectivity of hexamethylenediamine and corrode equipment
It is difficult to recover homogeneous catalysts, and the production cost of amorphous alloy catalysts is too high

Method used

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  • Method for preparing hexamethylene diamine by direct hydrogenation of adiponitrile under alkali-free conditions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 NiLa / MgO-Al 2 o 3 Catalyst preparation

[0016] According to the metering ratio of the catalytically active metal Ni to the oxide carrier, a certain mass of nickel nitrate and aluminum nitrate, and relative metering ratios of magnesium nitrate and lanthanum nitrate are dissolved in deionized water, and the concentration of aluminum ions is about 1mol / L. mixture. Then take anhydrous sodium carbonate with a stoichiometric ratio of 1.1 times relative to the metal ion and dissolve it in a certain amount of deionized water to prepare a sodium carbonate solution with pH=11. Then the above two clear solutions were dripped into a 250mL three-necked flask filled with 5-10mL deionized water at a rate of 1mL / min, that is, 3s / drop. During the dropwise addition, an oil bath was used to maintain a constant temperature of 45°C and vigorously stirred, at which point a light green precipitate gradually appeared. After the dropwise addition, the pH of the test mixture was 6...

Embodiment 2

[0017] Embodiment 2NiCe / BaO-Al 2 o 3 Catalyst preparation

[0018] According to the metering ratio of catalyst active metal Ni to the oxide carrier, a certain mass of nickel nitrate and aluminum nitrate, and relative metering ratio of barium nitrate and cerium nitrate are dissolved in deionized water, and the concentration of aluminum ions is about 1mol / L. mixture. Then take anhydrous sodium carbonate with a stoichiometric ratio of 1.1 times relative to the metal ion and dissolve it in a certain amount of deionized water to prepare a sodium carbonate solution with pH=11. Then the above two clear solutions were dripped into a 250mL three-necked flask filled with 5-10mL deionized water at a rate of 1mL / min, that is, 3s / drop. During the dropwise addition, an oil bath was used to maintain a constant temperature of 45°C and vigorously stirred, at which point a light green precipitate gradually appeared. After the dropwise addition, the pH of the test mixture was 6-7, and the pH...

Embodiment 3

[0019] Embodiment 3NiZr / SrO-Al 2 o 3 Catalyst preparation

[0020] According to the metering ratio of the catalytically active metal Ni to the oxide carrier, a certain mass of nickel nitrate and aluminum nitrate, and relative metering ratios of zirconium nitrate and strontium nitrate are dissolved in deionized water, and the concentration of aluminum ions is about 1mol / L. mixture. Then take anhydrous sodium carbonate with a stoichiometric ratio of 1.1 times relative to the metal ion and dissolve it in a certain amount of deionized water to prepare a sodium carbonate solution with pH=11. Then the above two clear solutions were dripped into a 250mL three-necked flask filled with 5-10mL deionized water at a rate of 1mL / min, that is, 3s / drop. During the dropwise addition, an oil bath was used to maintain a constant temperature of 45°C and vigorously stirred, at which point a light green precipitate gradually appeared. After the dropwise addition, the pH of the test mixture was...

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Abstract

The invention discloses a method for preparing hexamethylene diamine by direct hydrogenation of adiponitrile under alkali-free conditions. The method comprises the steps of using an alkaline earth metal oxide or rare earth metal oxide prepared by a coprecipitation method for modifying an aluminium trioxide-supported metallic nickel catalyst under a condition of no need of adding alkali or ammoniawater, directly hydrogenating an adiponitrile ethanol solution at a temperature of 60 to 200 DEG C, under pressure of 3 to 8 MPa, and obtaining high-qualityhexamethylene diamine through vacuum distillation of a resulting product. The method is suitable for using in batch tank reactors and also in continuous fixed bed reactors.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry and relates to a method for preparing hexamethylenediamine by direct hydrogenation of adiponitrile under alkali-free conditions. Background technique [0002] Both amino functional groups of hexamethylenediamine are highly reactive, which enables it to be used as a chemical intermediate in the production of numerous chemicals. Its industrial value is mainly reflected in the condensation of monomers or the reaction with other raw materials to produce condensation products, such as polycondensation with adipic acid or sebacic acid to prepare nylon 66 and nylon 610, and then synthesize other nylon resins, nylon fibers, and polyamide resin inks and other important civilian materials. In addition, hexamethylenediamine is also widely used in mining (oil field demulsifier), agriculture (pesticide), construction (concrete additive), etc. In addition, under ultraviolet irradiation, hexa...

Claims

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Application Information

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IPC IPC(8): C07C209/48C07C211/12B01J23/78B01J23/83B01J37/03B01J37/06
CPCB01J23/78B01J23/83B01J37/0036B01J37/03B01J37/06C07C209/48C07C211/12
Inventor 梁长海陈霄张玉莹邓天宇
Owner DALIAN UNIV OF TECH
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