Method for preparing organic diamine from organic amide and device thereof

A technology of organic amides and organic diamines, applied in the field of organic synthesis, can solve the problems of difficulty in obtaining high-purity 6-aminocapronitrile, high cost of large-scale production, low conversion rate of raw materials, etc., and achieve high selectivity of aminonitrile organic compounds , extended service life, and high purity

Active Publication Date: 2021-11-02
JIANGSU YANGNONG CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The caprolactam method uses caprolactam as a raw material to obtain 6-aminocapronitrile through catalytic amination, and then further catalyzes hydrogenation of 6-aminocapronitrile to obtain hexamethylenediamine. This method avoids the generation of diaminocyclohexane from the source and improves the Hexamethylenediamine product quality, but there are problems such as complicated process, long route and low conversion rate of raw materials, and the cost of large-scale production is high
[0003] CN111574400A discloses a method for separating the ammoniated dehydration product of caprolactam. In the separation method, the ammoniated dehydration product system is directly condensed without secondary heating, and continuous operation of reaction and product separation can be realized, and waste heat can be fully utilized. High separation efficiency, high production intensity and low separation energy consumption make the overall process more energy-saving; but this method is difficult to obtain high-purity 6-aminocapronitrile, which will affect the subsequent synthesis of hexamethylenediamine
[0005] CN112812020A discloses a method and device thereof for producing hexamethylenediamine from caprolactam. The method utilizes caprolactam aqueous solution as the diluent for the hydrogenation reaction of 6-aminocapronitrile, and does not need to add ethanol as the diluent, which reduces the generation of by-products, but After the method introduces water, the energy consumption is high, and the economic benefit is relatively poor.

Method used

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  • Method for preparing organic diamine from organic amide and device thereof
  • Method for preparing organic diamine from organic amide and device thereof
  • Method for preparing organic diamine from organic amide and device thereof

Examples

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preparation example Construction

[0311] The preparation method of catalyst A1 is carried out according to CN111659463A, except that in the molding step, a mold matching with catalyst A1 is used for molding to form catalyst A1 with a specific structure, other preparation methods are carried out according to CN111659463A.

[0312] Catalyst A2 to Catalyst A4 have the same structure and preparation method as Catalyst A1, except that the molar ratios of silicon, aluminum and phosphorus are 1:0.8:0.5, 1:0.8:0.8 and 1:0.8:1.6.

[0313] Catalyst B1

[0314] Catalyst B1 is a clover-shaped columnar catalyst. The clover-shaped catalyst includes a cylindrical body 1 and a protrusion 2, wherein the height of the cylinder is 5 mm, and the lobes outside the clover circle intersection are used as the protrusion 2, Specific as figure 1 As shown, the inside of the dotted line is marked as the main part of the catalyst, and the part outside the dotted circle is marked as the protruding part 2. The diameter of the dotted line c...

Embodiment 1

[0382] This embodiment provides a method for preparing hexamethylenediamine from caprolactam, such as Figure 8-10 As shown, the device used in the method includes a gasification unit 10, an ammoniation reaction unit 20, a first refining unit 30, a first adsorption unit 40, a hydrogenation reaction unit 50, a second refining unit 60 and a second refining unit 60 connected in sequence. Adsorption unit 70.

[0383] The gasification unit 10 includes a Venturi gasification device. The Venturi gasification device comprises a converging section 101, a throat 102 and a diverging section 103, the converging section 101 is provided with a first inlet 104, and the diverging section 103 is provided with a first gas outlet 105, so The throat 102 is provided with a second inlet. The Venturi gasification device also includes an external circulation pipeline connecting the diverging section 103 and the throat 102 . A material conveying device 106 is arranged on the external circulation pi...

Embodiment 2

[0399] This embodiment provides a method for preparing hexamethylenediamine from caprolactam, said method comprising the steps of:

[0400] (1) Isopropyl distearoyloxyaluminate (accounting for 20 ppm by weight of ammonia gas) is mixed with ammonia gas and preheated at 600° C. to superheat the ammonia gas to obtain a mixed gas.

[0401] The mixed gas and the first part of the organic amide in the liquid phase state at a temperature of 220 ° C are mixed and gasified at 500 ° C in the Venturi gasification device, and then passed into the first fixed-bed reactor (a total of 4 fixed-bed reactors in series) , counted as 4 sections of fixed-bed reactors, each section of fixed-bed reactors is filled with catalysts of the same weight), reacting at the first reaction temperature, the first reaction pressure and the first catalyst, to obtain the first reaction discharge;

[0402] The i-th reaction output and the i+1 part of the organic amide are passed into the i+1 section fixed-bed reac...

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Abstract

The invention provides a method for preparing organic diamine from organic amide and a device thereof, and the method comprises the following steps: (1) mixing and gasifying ammonia gas and organic amide to obtain a gasified material; carrying out ammoniation reaction on the gasified material under the action of an ammoniation catalyst to obtain a first reaction material; (2) carrying out first refining and first adsorption on the first reaction material to obtain an aminonitrile organic matter; (3) performing a hydrogenation reaction on the aminonitrile organic matter and hydrogen under the action of a hydrogenation catalyst, and obtaining a reacted material containing organic diamine; and (4) sequentially carrying out secondary refining and secondary adsorption on the reacted material to obtain an organic diamine product. According to the method, the organic amide is converted into the aminonitrile organic matter through the gas phase method, the aminonitrile organic matter is purified and then converted into the organic diamine through hydrogenation, the process is simple and easy to control, the yield and selectivity of the final organic diamine can be remarkably improved, and the economic benefits of the whole process are improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method and a device for preparing organic diamines from organic amides. Background technique [0002] Hexamethylenediamine is a key raw material in the nylon industry. It is often used to synthesize nylon 66 and nylon 610, and then to make nylon resin, nylon fiber and engineering plastics and other products. The industrial production method of hexamethylenediamine is mainly the catalytic hydrogenation of adiponitrile, which produces diaminocyclohexane, an impurity that has a great impact on the quality of nylon products, and is difficult to separate when producing hexamethylenediamine. At present, with the increasing capacity of caprolactam and the decreasing price, the caprolactam method is expected to be promoted industrially. The caprolactam method uses caprolactam as a raw material to obtain 6-aminocapronitrile through catalytic amination, and then further cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/50C07C211/12
CPCC07C209/50C07C211/12Y02P20/584
Inventor 王根林丁克鸿徐林王铖王刚吴健许越梅学赓汪洋聂庆超
Owner JIANGSU YANGNONG CHEM GROUP
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