Metal-based ionic liquid catalyst for preparing polyester through coupling reaction as well as preparation method and application of metal-based ionic liquid catalyst

A technology of ionic liquid and coupling reaction, which is applied in the field of metal-based ionic liquid catalyst and its preparation, can solve the problems of unsatisfactory activity, stability, selectivity and dispersion, and achieve good thermal and chemical stability, absorption Enhanced electrical capacity, non-flammable effect

Pending Publication Date: 2022-07-26
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention proposes a metal-based ionic liquid (MZF) catalyst for the preparation of polyester by coupling reaction and its preparation method and application. Unsatisfactory problems with sex and dispersion, while co-producing carbonates

Method used

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  • Metal-based ionic liquid catalyst for preparing polyester through coupling reaction as well as preparation method and application of metal-based ionic liquid catalyst
  • Metal-based ionic liquid catalyst for preparing polyester through coupling reaction as well as preparation method and application of metal-based ionic liquid catalyst
  • Metal-based ionic liquid catalyst for preparing polyester through coupling reaction as well as preparation method and application of metal-based ionic liquid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Step 1. Mix 0.5 mol of imidazole with 0.5 mol of dichloromethane, react at 70° C. for 12 h, wash with ethyl acetate, spin-evaporate, and vacuum dry to obtain intermediate Cl-I, respectively.

[0046] Step 2. N 2 Under the protection, 0.25mol of benzoic acid was added to the reactor equipped with the above-mentioned 0.5mol of intermediate Cl-I, stirred and dissolved, condensed and refluxed, the reaction time was controlled at 5h, washed with acetonitrile after the reaction was completed, rotary evaporated, and vacuum dried Afterwards, different kinds of intermediate Cl-II were obtained.

[0047]Step 3. Dissolve 1 mol of copper nitrate and 0.5 mol of intermediate Cl-II in 100 ml of deionized water, and sonicate. After the dissolution is completed, put it into a reaction kettle, and react at 61 °C for 3.5 h. After standing, suction filtration, and drying That is, the metal-based ionic liquid catalyst Cu-MZF-Cl is obtained, and the infrared spectrum is as follows image 3...

Embodiment 2

[0049] Step 1. Mix 0.5 mol of imidazole with 0.5 mol of dibromomethane, react at 80° C. for 20 h, wash with ethyl acetate, spin-evaporate, and vacuum dry to obtain intermediate Br-I, respectively.

[0050] Step 2. N 2 Under the protection, 0.75mol of benzoic acid was added to the reactor containing the above-mentioned 0.5mol of intermediate Br-I, stirred and dissolved, condensed and refluxed, and the reaction time was controlled at 11h. After the reaction, washed with acetonitrile, rotary evaporated, and vacuum dried Afterwards, different kinds of intermediates Br-II were obtained respectively.

[0051] Step 3. Dissolve 1 mol of ferric nitrate and 1 mol of intermediate Cl-II in 100 ml of deionized water, and sonicate. After the dissolution is completed, put it into a reaction kettle, and react at 67 ° C for 5.0 h. The metal-based ionic liquid catalyst Fe-MZF-Br was obtained, and the infrared spectrum is as follows image 3 shown.

Embodiment 3

[0053] Step 1. Mix 0.5 mol of imidazole with 0.5 mol of diiodomethane, react at 90° C. for 18 h, wash with ethyl acetate, spin-evaporate, and vacuum dry to obtain intermediates I-I, respectively.

[0054] Step 2. N 2 Under the protection, the 0.3mol benzoic acid added to the reactor equipped with the above-mentioned 0.5mol intermediate I-I was stirred and dissolved, condensed and refluxed, and the reaction time was controlled at 12h. Different kinds of intermediates I-II are obtained.

[0055] Step 3. Dissolve 1 mol of ferric nitrate and 1.5 mol of intermediate Cl-II in 100 ml of deionized water, and sonicate. After the dissolution is completed, put it into a reaction kettle, and react at 63 ° C for 4.0 h. After standing, suction filtration, and drying That is, the metal-based ionic liquid catalyst Mg-MZF-I is obtained, and the infrared spectrum is as follows image 3 shown.

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Abstract

The invention relates to a metal-based ionic liquid catalyst for preparing polyester by coupling reaction as well as a preparation method and application of the metal-based ionic liquid catalyst, the catalyst utilizes a unique cavity structure of MOF and high catalytic activity of ionic liquid, imidazole and benzoic acid are combined to prepare a novel MOF ligand, and then the novel MOF ligand reacts with nitrate to prepare an MZF catalyst. On one hand, the catalyst overcomes the defect that high-activity ionic liquid is difficult to disperse; on the other hand, the traditional MOF ligand structure is modified, and the MZF catalyst with a unique structure and catalytic performance is prepared, so that mutual synergistic catalysis of the ionic liquid and metal salt in MOF is realized, and the activity of the catalyst is further improved. The catalyst is used for the coupling reaction of cyclic carbonate and dicarboxylic ester to synthesize polyester and co-produce carbonate, the catalytic system has the characteristics of strong designability, high thermal stability, easy dispersion and the like, the catalytic system of dangerous elements such as heavy metals and the like is avoided, the catalyst is green and safe, the reaction process is stable and controllable, and the catalyst has industrial application value.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a metal-based ionic liquid catalyst for preparing polyester by coupling reaction, and a preparation method and application thereof. [0002] technical background [0003] As a common plastic, polyester is used in many fields such as product packaging, electronic appliances, medical and health, construction, automobiles and other fields. It has high thermodynamic stability and mechanical properties, especially high molecular weight polyester has similar properties to high density polyethylene, and has better comprehensive properties. Moreover, the cost of synthetic raw materials is also low, and it has good application and development prospects. [0004] Common preparation methods of polyester are melt polycondensation and transesterification. However, with the global restrictions and in-depth development of carbon dioxide emissions, cyclic carbonates, as an important product o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/82C08G63/83C08G83/00
CPCC08G83/008C08G63/16C08G63/83C08G63/826
Inventor 鄢文祥王海玥蒋泽众郭立颖宋晓慧李权峰叶鑫鑫曹安崎郭润春陈欣月尹妍
Owner SHENYANG POLYTECHNIC UNIV
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