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Preparation method of hexamethylenediamine

A technology of hexamethylene diamine and adiponitrile, which is applied in the field of preparation of hexamethylene diamine, can solve the problems of prone to spontaneous combustion, difficult product separation, environmental pollution, etc., and achieves the effects of easy recovery and recycling and high purity

Inactive Publication Date: 2018-03-16
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems of this method are: Raney Ni is very active in nature, and it is prone to spontaneous combustion when exposed to the air; it is difficult to separate the products after the reaction; a large amount of strong alkaline waste liquid is discharged during the production process, causing environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Catalyst preparation:

[0020] Mix 10.2g of 4M aqueous sodium hydroxide solution, 9.6g of aluminum nitrate nonahydrate, 1.5g of pyromellitic acid and 60g of deionized water, and pour the mixture into a stainless steel reactor, react at 210°C for 24 hours, and then react The mixture was cooled to room temperature, filtered, and the solid filter residue powder product was placed in deionized water, refluxed at 100°C for 10 hours, cooled, filtered, and dried at room temperature to obtain a crystal metal organic framework compound aluminum pyromellitic acid.

[0021] Dissolve 1.07g, 0.94g and 1.29g of nickel acetate in 5ml of deionized water respectively, then add 0.35g, 0.3g and 0.4g of nickel nitrate respectively, then add 0.8g of the above-mentioned newly prepared crystalline organometallic compound, and stir at room temperature 12-24h, dry, filter, and then dry at 100°C for 24h. The obtained solid was calcined in the air, and the calcining method was as follows: the va...

Embodiment 2

[0023] Add 10g adiponitrile, 20g absolute ethanol and 0.2g catalyst Ni-MgO-MIL-1 into a 100mL autoclave, seal the autoclave, replace the air in the autoclave with hydrogen (0.2-0.4MPa) for 3-5 times, Place in heating mantle. After the temperature in the kettle rose to 75°C, add hydrogen to 2 MPa, turn on the magnetic stirrer, and start timing the reaction. After reacting for 3 hours, cool, filter and separate the catalyst and the mixed solution, put the supernatant into the still, and first recover the solvent ethanol by distillation under normal pressure (the temperature at the top of the tower is 78.3° C); The internal vacuum was maintained at 740mmHg-745mmHg (residual pressure 20mmHg), and fractions at 100±5°C were collected and analyzed by gas chromatography, and 7.5g of hexamethylenediamine was harvested, with a yield of 70% and a purity of 99%.

Embodiment 3

[0025] Add 10g adiponitrile, 20g absolute ethanol and 0.35g catalyst Ni-MgO-MIL-2 into a 100mL autoclave, seal the autoclave, replace the air in the autoclave with hydrogen (0.2-0.4MPa) for 3-5 times, Place in heating mantle. After the temperature in the kettle rose to 75°C, add hydrogen to 2 MPa, turn on the magnetic stirrer, and start timing the reaction. After reacting for 3 hours, cool, filter and separate the catalyst and the mixed solution, put the supernatant into the still, and first recover the solvent ethanol by distillation under normal pressure (the temperature at the top of the tower is 78.3° C); The internal vacuum was maintained at 740mmHg-745mmHg (residual pressure 20mmHg), and the fraction at 100±5°C was collected and analyzed by gas chromatography, and 7.2g of hexamethylenediamine was harvested, with a yield of 72.63% and a purity of 99%.

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Abstract

The invention discloses a preparation method of hexamethylenediamine. Hexane dinitrile is used as a raw material, and a nano-nickel and magnesium oxide composite material is used as a catalyst to prepare the hexamethylenediamine through liquid phase hydrogenation. The preparation method of the hexamethylenediamine comprises the following steps: dipping a porous carrier by using nickel acetate andmagnesium nitrate aqueous solutions at different concentrations at first, and carrying out in-situ reduction to obtain an immobilized nickel and magnesium oxide based composite catalyst under different conditions; adding raw materials, the catalyst and a solvent in a reaction kettle in proportion, sealing the reaction kettle, removing air in the kettle by a hydrogen substitution method, starting aheating power supply, applying set pressure to hydrogen after the temperature in the kettle is raised to the set reaction temperature, then starting a magnetic stirrer, and beginning to time reaction; and after the reaction is finished, filtering out the catalyst, and distilling and separating under reduced pressure. The yield of a target product is high, the yield of the hexamethylenediamine isgreater than 70%, and the solvent and the catalyst are recyclable.

Description

technical field [0001] The invention belongs to the technical field of petrochemical catalysis, and in particular relates to a preparation method of hexamethylenediamine. Background technique [0002] Hexamethylenediamine is an important organic chemical intermediate, mostly used as a raw material for the synthesis of polyamide, such as for the synthesis of nylon-66 salt and nylon 610, and also used as a curing agent and crosslinking agent for urea resin and epoxy resin . At present, with the development of the synthetic fiber industry, the demand for hexamethylenediamine compounds is increasing worldwide, and the market demand is relatively large. [0003] At present, hexamethylenediamine is mainly produced industrially through the liquid-phase hydrogenation of adiponitrile catalyzed by Raney Ni. Domestic hexamethylenediamine production equipment and technologies are mainly imported from abroad, such as the process technology route imported by Henan Shenma Group from Japa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/12B01J31/26
Inventor 李俊王振卫
Owner SHANGHAI INST OF TECH
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