Immobilized Catalysts of Silane-Coupled Molecular Sieves and Double Salt Ionic Liquids

A silane coupling, ionic liquid technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc. Insufficient selectivity

Active Publication Date: 2020-07-07
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Purpose of the invention: The technical solution of the present invention is to overcome the shortcomings of the existing technology that cannot realize the fixed-bed continuous catalytic conversion of carbon dioxide and the separation and treatment of traditional catalysts, the catalytic efficiency and selectivity are not high enough, and the service life is short. Preparation method of immobilized catalyst of silane coupling molecular sieve and double salt ionic liquid

Method used

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  • Immobilized Catalysts of Silane-Coupled Molecular Sieves and Double Salt Ionic Liquids
  • Immobilized Catalysts of Silane-Coupled Molecular Sieves and Double Salt Ionic Liquids
  • Immobilized Catalysts of Silane-Coupled Molecular Sieves and Double Salt Ionic Liquids

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preparation example Construction

[0034] Preparation method of the present invention carries out according to the following steps:

[0035] 1) First, use methylimidazole or alkylimidazole and halogenated alkyl alcohol / acid to stir at a temperature of 70°C~90°C, and react for 10-24 hours to prepare a functionalized ionic liquid with active groups. Washing, rotary evaporation, and purification for later use;

[0036] 2) Mix the functionalized ionic liquid and Lewis acid with a molar ratio of 1:2 into a three-necked flask, stir and react at 100°C, and continue the reaction for 15 minutes when the system changes from the original solid-liquid two-phase to a homogeneous phase h to obtain the double salt ionic liquid.

[0037] 3) Weigh molecular sieve and silane with a mass ratio of 1:1 and add them into a round bottom flask with a reflux condenser, use toluene as a solvent, react at 110°C for 24 hours, and remove the toluene solvent by rotary evaporation, the sample Dry in a vacuum oven for 12 h to obtain silane mo...

Embodiment 1

[0049] Put 9.63 mL of N-methylimidazole in a 100 mL three-neck flask, add 9.5 g of chloroacetic acid in three batches, and after the chloroacetic acid is completely dissolved, place the reaction in a water bath at 70°C for 10 h to obtain light yellow The liquid was poured into a beaker while it was hot and washed repeatedly with ether three times, placed in a vacuum drying oven at 80°C and -0.09 MPa for 12 h under reduced pressure to obtain 1-carboxyethyl-3-methylimidazolium chloride ionic liquid [CeMIM ] Cl, yield 91%.

[0050] Mix 6.65 g of 1-carboxyethyl-3-methylimidazolium chloride ionic liquid [CeMIM]Cl and 16.96 g of ZnBr2 into a round-bottomed flask with reflux condensation, and stir the reaction at 100 °C until the system consists of When the original solid-liquid two-phase transformation into a homogeneous phase, continue to react for 15 h to obtain the double salt ionic liquid [CeMIM]Cl / (ZnBr2)2.

[0051] Mix 5 g molecular sieve MCM-22 and 5 g 3-chloropropyltriethox...

Embodiment 2

[0055] Mix 24 mL of N-methylimidazole and 20 mL of 2-chloroethanol into a round-bottomed flask with a reflux condenser, under nitrogen protection, stir in a water bath at 80°C for 24 h, stop the reaction, and obtain a light yellow liquid Repeated extraction with ether 4 times, placed in a vacuum drying oven at 80°C, -0.09 MPa for 12 h under reduced pressure to obtain 1-(2-hydroxyethyl)-3-methylimidazolium ionic liquid [HeMIM]Cl, The yield was 94%.

[0056] Mix 6.0 g of chlorinated 1-(2-hydroxyethyl)-3-methylimidazolium ionic liquid [HeMIM]Cl and 16.33 g of ZnBr2 into a round-bottomed flask with reflux condensation, and stir the reaction at 100°C , when the system changed from the original solid-liquid two-phase to homogeneous, continue the reaction for 15 h to obtain the double salt ionic liquid [HeMIM]Cl / (ZnBr2)2.

[0057] Mix 5 g molecular sieve MCM-22 and 5 g 3-chloropropyltriethoxysilane (CPTES) into a round bottom flask with a reflux condenser, use toluene as solvent, an...

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Abstract

The invention belongs to the technical field of catalysts, and relates to a preparation method of a solid-supported catalyst of a silane coupling molecular sieve and a double salt ionic liquid. First, the equal mass of molecular sieve and silane were reacted in toluene solvent at 110°C for 24 h, and the toluene solvent was removed by rotary evaporation, and the sample was placed in a vacuum drying oven to dry for 12 h to obtain silane molecular sieve; then functionalized ionic liquid and Lewis acid Reaction, prepare double salt ionic liquid, mix it with silane molecular sieve, react in acetonitrile solvent for 24 h, then remove acetonitrile by rotary evaporation, extract the obtained sample with dichloromethane Soxhlet for 24 h, and then put it in a vacuum drying oven to dry for 8 h Finally, the target product silane coupling molecular sieve / double salt ionic liquid solid-supported catalyst is obtained. Finally, the immobilized catalyst was blended with a small amount of silica sol, squash powder, etc., and a catalyst sample was prepared using a catalyst molding extrusion device. After drying at 100°C for 10 h, it was used for continuous catalytic conversion of CO2 and propylene oxide in a fixed bed, and synthesized High purity propylene carbonate product.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a method for preparing a solid-supported catalyst of a silane-coupled molecular sieve and a double salt ionic liquid, in particular to a catalyst for preparing propylene carbonate by continuously catalyzing the cycloaddition reaction of carbon dioxide and propylene oxide . Background technique [0002] Alkylene oxide is the second largest industrial chain downstream of olefins. The by-product of its industrial production process is mainly CO2, and about 200-300 kg of CO2 is produced per ton of epoxide produced. Studies have shown that the carbonylation coupling reaction of CO2 and epoxy compounds to prepare cyclic carbonates is a reaction in line with the principle of "green and sustainable development". It is not only an effective way to achieve energy saving and emission reduction and low-carbon economic development, but also opens up A new route of non-petroleum raw materials...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26B01J31/02C07D317/36
Inventor 郭立颖金先超邓莉莉吴昊殷龙珠齐浩马恩庆王宏宇王浩志
Owner SHENYANG POLYTECHNIC UNIV
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