Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of treatment method of ion exchange resin catalyst for preparing caprolactam

An ion exchange resin, caprolactam technology, applied to the preparation of lactam, chemical instruments and methods, physical/chemical process catalysts and other directions, can solve the problems of caprolactam cost increase, deactivation, product blockage, etc., to achieve product specifications controllable, Long-lived, simple-to-step effect

Active Publication Date: 2022-04-15
CHINA TIANCHEN ENG
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, caprolactam oligomers are formed when ion exchange resins are used as catalysts, which leads to an increase in the cost of caprolactam
Moreover, as the reaction progresses, the pore structure of the resin catalyst will be blocked by the product, causing its active groups to be covered and deactivation occurs.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of treatment method of ion exchange resin catalyst for preparing caprolactam
  • A kind of treatment method of ion exchange resin catalyst for preparing caprolactam
  • A kind of treatment method of ion exchange resin catalyst for preparing caprolactam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In the embodiment of the present invention, the treatment method for the strong acid ion exchange resin used to prepare caprolactam, the specific steps are as follows:

[0035] (1) Configure metal ion aqueous solution, Cu(NO 3 ) 2 The solution concentration is 0.1mol / ;

[0036] (2) Put 1000g NKC-9 ion exchange resin into 1L metal ion aqueous solution, take it out after stirring for 1h, and wash until neutral;

[0037] (3) configuration sodium dodecylbenzene sulfonate aqueous solution, concentration is 0.1g / L;

[0038] (4) immerse 1000 g of the resin catalyst obtained in step (2) into 10 L of the treatment liquid obtained in step (3), stir at 60° C. for 2 hours, then wash the resin catalyst to neutrality, and dry at 120° C. for 4 hours;

[0039] (5) configure the dimethyl sulfoxide solution of cyclohexanone oxime, the concentration of cyclohexanone oxime is 150g / L;

[0040] (6) the resin catalyst 100g that step (4) gained is placed in 100ml fixed bed, heating and kee...

Embodiment 2

[0044] In the embodiment of the present invention, the treatment method of the strong acid type ion exchange resin, the specific steps are as follows:

[0045] (1) configure metal ion aqueous solution, Zn(NO 3 ) 2 The solution concentration is 0.1mol / ;

[0046] (2) Put 1000g Amberlyst-15 ion exchange resin into 1.5L metal ion aqueous solution, take it out after stirring for 1h, and wash until neutral;

[0047] (3) configuration sodium dodecylbenzene sulfonate aqueous solution, concentration is 1.5g / L;

[0048](4) Immerse 1000 g of the resin catalyst obtained in step (2) into 2 L of the treatment liquid obtained in step (3), stir at 60° C. for 2 hours, then wash the resin catalyst to neutrality, and dry at 120° C. for 4 hours;

[0049] (5) configure the toluene solution of cyclohexanone oxime, the concentration of cyclohexanone oxime is 500g / L;

[0050] (6) the resin catalyst 100g that step (4) gained is placed in 100ml fixed bed, heating and keeping reactor temperature is ...

Embodiment 3

[0054] In the embodiment of the present invention, the treatment method of the strong acid type ion exchange resin, the specific steps are as follows:

[0055] (1) Configure metal ion aqueous solution, RuCl 3 The solution concentration is 0.01mol / ;

[0056] (2) Put 1000g NKC-9 ion exchange resin into 1L metal ion aqueous solution, take it out after stirring for 1h, and wash until neutral;

[0057] (3) configuration cetyltrimethylammonium bromide aqueous solution, concentration is 1g / L;

[0058] (4) immerse 1000 g of the resin catalyst obtained in step (2) into 10 L of the treatment liquid obtained in step (3), stir at 60° C. for 2 hours, then wash the resin catalyst to neutrality, and dry at 120° C. for 4 hours;

[0059] (5) configure the toluene solution of cyclohexanone oxime, the concentration of cyclohexanone oxime is 250g / L;

[0060] (6) Place the resin catalyst 100g obtained in step (4) in a fixed bed, heat and keep the reactor temperature at 100°C, and the residence ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a treatment method for preparing caprolactam ion exchange resin catalyst, comprising the following steps: (1) immersing the strong acid type cation exchange resin in a specific metal salt solution, and starting to stir; The resin obtained in step (1) is cleaned to neutrality, and then the resin is put into the chemical treatment solution, and the stirring is started; 3) The resin catalyst obtained in step (2) is cleaned to neutrality, and dried; 4) The obtained resin in step (3) is The resin catalyst is placed in a fixed-bed reactor, and a cyclohexanone oxime solvent is passed into the reactor, and heated to a certain temperature to obtain caprolactam. The invention solves the problems of low selectivity and easy deactivation of the catalyst in the preparation of caprolactam by using the resin catalyst in the previous research. The invention has simple operation method, mild reaction conditions and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of chemical catalysts, in particular to a treatment method of an ion exchange resin catalyst used for liquid-phase Beckmann rearrangement to prepare caprolactam. Background technique [0002] Caprolactam is an important chemical raw material and an important monomer for the synthesis of polymers such as nylon. Caprolactam is mainly produced by the Beckmann rearrangement reaction of cyclohexanone oxime. The Beckmann rearrangement reaction is an acid-catalyzed rearrangement reaction in which the reactant oxime is rearranged to an amide under the catalysis of an acid. Acids that can catalyze the Beckmann rearrangement reaction include acetic acid, hydrochloric acid and acetic anhydride, sulfuric acid, and solid acids. At present, the synthesis of caprolactam in industry is mainly through the rearrangement reaction of cyclohexanone oxime under the action of concentrated sulfuric acid or oleum, and then using ammonia to ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D201/04B01J31/08
CPCC07D201/04B01J31/08Y02P20/52
Inventor 庄大为刘文赵斌杨克俭王聪
Owner CHINA TIANCHEN ENG