A kind of preparation method of hexamethylenediamine

A technology of hexamethylenediamine and cyclohexanediol, which is applied in the field of preparation of hexamethylenediamine, can solve the problems of complex technology, patent technology transfer fees, high one-time construction investment, and large safety risks, and achieve easy-to-obtain reaction media, The production process is green and has obvious advantages

Active Publication Date: 2017-03-15
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complexity of the technology and the high degree of monopoly at present, the patent technology transfer fee and the one-time construction investment are relatively high, and the project is required to have sufficient and cheap 1,3-butadiene resources, which largely limits the The popularization and application of the process
[0008] Most of the methods of using adiponitrile to prepare hexamethylenediamine involve highly toxic raw materials, such as hydrocyanic acid, sodium cyanide and other substances as raw materials, so there are problems such as high safety risks

Method used

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  • A kind of preparation method of hexamethylenediamine
  • A kind of preparation method of hexamethylenediamine
  • A kind of preparation method of hexamethylenediamine

Examples

Experimental program
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Embodiment 1

[0044] Preparation of 1-hexadecyl-3-methylimidazolium decapolytungstate quaternary ammonium salt: Weigh 33.03g of sodium tungstate into a beaker filled with 100mL of water to dissolve, stir magnetically at 60°C, and use 3mol / L hydrochloric acid to adjust its pH value to about 2, then slowly add dropwise a 10mL ethanol solution containing 15.51g of 1-hexadecyl-3-methylimidazolium bromide after heating up to 90°C, and the solution immediately appears white turbid. After the dropwise addition, the reaction was continued at 90°C for 0.5h. After the reaction, the white or light yellow solid was obtained by filtration, washed with water and ethanol, and dried in vacuum.

[0045] Preparation of 1,2-cyclohexanediol: At room temperature, add 1.05g of 1-hexadecyl-3-methylimidazole decapolytungstate quaternary ammonium salt catalyst, 1.05g of phosphoric acid and 20.51g of Cyclohexene was stirred vigorously, and 34.01 g of 30% hydrogen peroxide was slowly added dropwise. At the same time...

Embodiment 2-12

[0051] Except that the corresponding conditions in Example 1 were replaced by the experimental conditions in the following table, the reaction was basically carried out according to the same reaction conditions as in Example 1. The yield data obtained are shown in Table 1.

[0052] Table I

[0053]

[0054] Wherein, in the process of preparing 1,2-cyclohexanediol, catalyst A is the same as that described in the first paragraph of Example 1, using 1-hexadecyl-3-methylimidazolium bromide to prepare 1 -hexadecyl-3-methylimidazole decapolytungstate quaternary ammonium salt; Catalyst B is to replace the 1-hexadecyl-3-methylimidazolium bromide in Example 1 with butyl trimethyl deca Polytungstic acid bromide is prepared as raw material; catalyst C is to replace 1-hexadecyl-3-methylimidazolium bromide in Example 1 with N-hexadecylpyridine decapolytungstate bromide as raw material prepared.

[0055] According to the above examples, it can be seen that the industrialized 1,6-hexan...

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Abstract

The invention discloses a preparation method of hexamethylenediamine. The method is used for preparing 1, 6-hexamethylenediamine by virtue of carrying out ammoniation and catalytic hydrogenation on 1, 6-adipaldehyde. The method is simple in process, low in cost, high in yield, low in energy consumption and free from industrial three wastes.

Description

technical field [0001] The present invention relates to a kind of preparation method of hexamethylenediamine, specifically, the present invention relates to a kind of method that makes adipaldehyde ammoniation catalytic hydrogenation to prepare hexamethylenediamine, more specifically, adipaldehyde can be obtained by cyclohexane Alkenes are the starting materials and are prepared by catalytic oxidation. The method has the advantages of simple process, low cost, high yield, low energy consumption and no industrial wastes. Background technique [0002] Hexamethylenediamine is a colorless flaky crystal with an ammonia smell, with a boiling point of 204-205°C and a melting point of 41-42°C. Hexamethylenediamine is the main raw material for the manufacture of polyamide (nylon) fibers and resins. Nylon 66 can be produced by condensation reaction of hexamethylenediamine and adipic acid to produce nylon 66 salt solution, and then concentrated and polycondensed. [0003] At present...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/12C07C209/26
Inventor 张英伟苏思正张敏生曹亚林崔冰冰
Owner BEIJING RISUN TECH CO LTD
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