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Polymer-supported dual-core acid ion liquid catalyst and preparation and application thereof

A technology of ionic liquids and polymers, applied in the preparation of organic compounds, catalysts of organic compounds/hydrides/coordination complexes, catalysts for physical/chemical processes, etc. Easy to lose components and other problems, to achieve the effect of broad industrial application prospects, fast mass transfer rate, and simple preparation method

Inactive Publication Date: 2017-08-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, silica gel has strong adsorption, is porous and is rich in active groups Si-OH, but it often needs to introduce expensive silane coupling agent, which is not conducive to large-scale production; molecular sieves have large specific surface area and active group Si-OH It is easy to realize ionic liquid bonding, but the hydrothermal stability is low, which may affect the actual use effect; activated carbon has large porosity, strong adsorption, and is cheap and easy to obtain, but ionic liquid is immobilized on its surface by physical adsorption. Active components are easy to lose and have poor stability; organic polymer materials mainly include polystyrene resins, polyesters, etc. It has high compatibility with the reaction system and is an excellent carrier

Method used

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  • Polymer-supported dual-core acid ion liquid catalyst and preparation and application thereof
  • Polymer-supported dual-core acid ion liquid catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of polymer-loaded double nucleic acid ionic liquid:

[0027] (1) Preparation of polychloromethylstyrene microspheres

[0028] Add 6g of vinylbenzyl chloride, 2g of styrene, 3.2g of divinylbenzene, 0.1g of polyvinyl alcohol, 0.7g of azobisisobutyronitrile and 4.5g of n- Heptane, N 2 Under protection, reflux reaction at 70°C for 8 hours, the obtained product is suction filtered, washed, dried, and then sieved to obtain 20-200 mesh polymer microspheres;

[0029] (2) Polychloromethylstyrene microspheres loaded with ionic liquids

[0030] ① Using acetonitrile as a solvent, mix the above polymer carrier with bis(2-chloroethyl)amine at a mass ratio of 1.0:1.0, heat to 50°C, and react with magnetic stirring for 12 hours. Wash with acetonitrile, methanol, and ethanol, and dry in vacuum;

[0031] ②Using DMF as solvent, mix the product obtained in step ① with benzimidazole at a mass ratio of 1.0:1.0, heat to 75°C, and react with magnetic stirring for 24 ...

Embodiment 2

[0035] The preparation method of polymer-loaded double nucleic acid ionic liquid:

[0036] (1) Preparation of polychloromethylstyrene microspheres

[0037] Add 6g of vinylbenzyl chloride, 2g of styrene, 3.2g of divinylbenzene, 0.1g of polyvinyl alcohol, 0.7g of azobisisobutyronitrile and 6.7g of n- Heptane, N 2 Under protection, reflux reaction at 60°C for 8 hours, the obtained product can be obtained after suction filtration, washing, drying, and sieving to obtain 20-200 mesh polymer microspheres;

[0038] (2) Polychloromethylstyrene microspheres loaded with ionic liquids

[0039] ① Using acetonitrile as a solvent, mix the above polymer carrier with bis(2-chloroethyl)amine at a mass ratio of 1.0:1.0, heat to 40°C, and react with magnetic stirring for 12 hours. Wash with acetonitrile, methanol, and ethanol, and dry in vacuum;

[0040] ② Using DMF as a solvent, mix the product obtained in step ① with benzimidazole at a mass ratio of 1.0:1.0, heat to 90°C, and react with magne...

Embodiment 3

[0044] The preparation method of polymer-loaded double nucleic acid ionic liquid:

[0045] (1) Preparation of polychloromethylstyrene microspheres

[0046] Add 6g of vinylbenzyl chloride, 2g of styrene, 3.2g of divinylbenzene, 0.1g of polyvinyl alcohol, 0.7g of azobisisobutyronitrile and 6.7g of n- Heptane, under the protection of N2, reflux reaction at 80°C for 8 hours, the obtained product is suction filtered, washed, dried, and then sieved to obtain polymer microspheres of 20-200 mesh;

[0047] (2) Polychloromethylstyrene microspheres loaded with ionic liquids

[0048] ①Using acetonitrile as solvent, mix the above polymer carrier with bis(2-chloroethyl)amine at a mass ratio of 2.0:1.0, heat to 60°C, and react with magnetic stirring for 12 hours. Wash with acetonitrile, methanol, ethanol, etc., and dry in vacuum;

[0049] ② Using DMF as a solvent, mix the product obtained in step ① with benzimidazole at a mass ratio of 1.0:1.0, heat to 90°C, and react with magnetic stirri...

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Abstract

The invention discloses a polymer-supported dual-core acid ion liquid catalyst and preparation and application thereof. According to the polymer-supported dual-core acid ion liquid catalyst, vinylbenzyl chloride and vinyl benzene serve as polymeric monomers, divinyl benzene serve as cross-linking agent, polymers obtained through free radical polymerization serve as carriers, bis(2-chloroethyl) amine, benzimidazole, 1, 3-propane sultone and concentrated sulfuric acid or trifluoromethanesulfonic acid serve as the raw materials, and through a bonding method, effective immobilization of ionic liquid onto polymeric microspheres can be achieved. The polymer-supported dual-core acid ion liquid catalyst blends the advantages of the ionic liquid and polymers and has the advantages of being large in specific surface area, adjustable in pore structure, high in hydrophobicity, simple in preparation method, high in catalytic activity and mass transfer rate, good in selectivity, high in stability, easy to recover and separate, environmentally friendly, broad in industrialized application prospect and the like. When applied to esterification reaction of various acids and alcohols, the polymer-supported dual-core acid ion liquid catalyst can achieve good effects.

Description

technical field [0001] The invention relates to the technical field of synthesis of catalytic materials for esterification, in particular to a polymer-supported dual nucleic acid ionic liquid catalyst and its preparation and application. Background technique [0002] Esterification reaction is an important organic synthesis reaction, which generally refers to the reaction of alcohol and carboxylic acid or oxygen-containing inorganic acid to generate ester and water. It is widely used in the production of perfumes, dyes, solvents and pharmaceutical products. The esterification reaction is a reversible reaction and the reaction speed is slow, and the commonly used catalysts are protonic acids, such as concentrated sulfuric acid and hydrofluoric acid. Although such traditional catalysts have high catalytic activity, they have problems such as strong corrosion, serious pollution, and difficulty in separating the catalyst from the reaction system. In recent years, with extensive...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J32/00C07C67/08C07C69/14C07C69/24C08F212/14C08F212/08C08F212/36
CPCB01J31/0282B01J31/06C07C67/08C08F212/14C07C69/14C07C69/24C08F212/08C08F212/36
Inventor 邱挺凌笑媚杨金杯李玲叶长燊王晓达黄智贤王红星杨臣
Owner FUZHOU UNIV
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