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Catalyst for preparing 6-aminocapronitrile from cyclohexanone-oxime and application of catalyst

A technology for cyclohexanone oxime and aminocapronitrile is applied in the field of catalysts for preparing 6-aminocapronitrile from cyclohexanone oxime, which can solve the problems of less investment, more three wastes, short technological process, etc., and saves investment and reduces energy consumption. , reduce the effect of the process

Pending Publication Date: 2022-07-22
舟山柏川管理咨询合伙企业(有限合伙)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no patent on the preparation of 6-aminocapronitrile from cyclohexanone oxime. Although patents such as US2234566 and FR1573490 mention the technology of using caprolactam to prepare 6-aminocapronitrile, the rearrangement of cyclohexanone oxime to obtain caprolactam requires a complicated refining process. , large investment, high energy consumption, and many wastes
[0003] One-step preparation of 6-aminocapronitrile by cyclohexanone oxime has the characteristics of short technological process and less investment, but there is no relevant technology at present, so a preparation process for preparing 6-aminocapronitrile by one-step method of cyclohexanone oxime is invented And its catalyst, the industrial prospect is good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Preparation of catalyst based on titanium silicon molecular sieve

[0026] Using silica sol as the silicon source, titanium tetrachloride or butyl titanate as the titanium source, and tetrapropylammonium bromide as the template agent, a homogeneous glue solution is prepared at room temperature, and the phosphate is composed of 20-50 parts according to the catalyst. , 1-20 parts of metal oxide, 30-60 parts of molecular sieve, add anhydrous magnesium phosphate and titanium dioxide, mix and stir evenly, then put into an autoclave, and crystallize at 150-200 ℃ autogenous pressure for 5-7 days to obtain solid powder After being filtered, washed and dried, calcined at 500-600° C. for 5-15 hours to obtain catalyst A whose molecular sieve is a titanium-silicon molecular sieve.

Embodiment 2

[0027] Example 2 Preparation of catalyst based on all-silicon molecular sieve

[0028] Add ethyl silicate, tetrapropyl ammonium hydroxide solution and ethanol to the reaction kettle to form a gel-sol mixture raw material, which is composed of 20-50 parts of phosphate, 1-20 parts of metal oxide, and 30-60 parts of molecular sieve according to the catalyst. Add barium phosphate and titanium dioxide in a proportion of parts, crystallize at 100-170 ° C for 2-5 d, wash with water to pH 7.5-8.5, and dry; roast at 500-600 ° C for 5-15 hours to prepare all-silicon molecular sieve-based catalyst B.

Embodiment 3

[0029] Example 3 Preparation of catalyst based on ZSM-5 molecular sieve

[0030] A certain amount of aluminum isopropoxide (AIP) was dissolved in an aqueous solution containing a templating agent, stirred by a magnetic stirrer for several hours until dissolved, then ethyl orthosilicate (TEOS) was added, and the raw material mixture was kept at room temperature. Stir overnight to make it completely hydrolyzed, and add anhydrous magnesium phosphate and titanium dioxide according to the ratio of catalyst composition of 20-50 parts of phosphate, 1-20 parts of metal oxide, and 30-60 parts of molecular sieve. The template agent is one or more of tetrapropylammonium hydroxide (TPAOH), n-butylamine (n-BTA) and ethanol (Ethanol), and the initial gel ratio is 20-50Mg 3 (PO 4 ) 2 : 1-20TiO 2 : 1-5Al 2 O 3 : 30-60SiO 2 : 5-15 TPAOH: 3-8 n-BTA: 2-5 Ethanol: 2500 H 2 O. The raw material mixture was placed in a crystallization kettle with polytetrafluoroethylene, reacted at 170 °C fo...

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PUM

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Abstract

The invention discloses a catalyst for preparing 6-aminocapronitrile from cyclohexanone-oxime and application of the catalyst, and the catalyst is prepared from the following components in parts by mass: 20-50 parts of phosphate, 1-20 parts of metal oxide and 30-60 parts of molecular sieve. In the presence of a catalyst, gas-phase cyclohexanone-oxime and ammonia gas react at the reaction temperature of 320-450 DEG C under the pressure of 0-1.0 MPa, the weight space velocity of the cyclohexanone-oxime is 0.1-10h <-1 >, cyclohexanone-oxime steam and hot ammonia gas are mixed according to the mass ratio of (1: 2)-(1: 20), the conversion per pass of the cyclohexanone-oxime is 60-70%, and the selectivity of the 6-aminocapronitrile reaches more than 95%.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a method for preparing 6-aminocapronitrile from cyclohexanone oxime, in particular to a catalyst for preparing 6-aminocapronitrile from cyclohexanone oxime and its application. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate, which can be used to produce 1,6 hexanediamine by complete hydrogenation, and 1,6 hexanediamine can be used to produce the polymer nylon 66. At present, 6-aminocapronitrile is mainly obtained by partial hydrogenation of 1 and 6 adiponitrile, such as patents CN1238334C, CN101309897B, or by hydroformylation of pentene nitrile, such as patent CN1100752C. There is no patent for preparing 6-aminocapronitrile from cyclohexanone oxime. Although patents US2234566, FR1573490, etc. mentioned the technology of using caprolactam to prepare 6-aminocapronitrile, but cyclohexanone oxime is rearranged to obtain caprola...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J29/40B01J29/03C07C253/00C07C255/24
CPCB01J29/89B01J29/405B01J29/03C07C253/00C07C255/24
Inventor 陈曼柏虞新建潘利李珊陈天然
Owner 舟山柏川管理咨询合伙企业(有限合伙)