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A kind of quaternary phosphonium type deep eutectic ionic liquid catalyzes the method for coupling carbon dioxide and epoxide to prepare cyclic carbonate

A cyclic carbonate, ionic liquid technology, applied in chemical instruments and methods, catalytic reactions, chemical/physical processes, etc., can solve the problems of further improvement of catalytic activity and harsh catalytic reaction conditions, and achieve excellent universality and The effect of recycling performance, avoiding secondary emission problems, and good prospects for industrial application

Active Publication Date: 2021-04-27
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above catalytic systems still have the problem of harsh catalytic reaction conditions (high temperature, high pressure), and the catalytic activity needs to be further improved.
Based on the above reports, explore and develop a new type of green deep eutectic ionic liquid, so that it can efficiently catalyze CO under mild (or normal temperature and pressure) conditions. 2 The synthesis of metal-free ionic liquid catalysts for cyclic carbonates is still a great challenge

Method used

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  • A kind of quaternary phosphonium type deep eutectic ionic liquid catalyzes the method for coupling carbon dioxide and epoxide to prepare cyclic carbonate
  • A kind of quaternary phosphonium type deep eutectic ionic liquid catalyzes the method for coupling carbon dioxide and epoxide to prepare cyclic carbonate
  • A kind of quaternary phosphonium type deep eutectic ionic liquid catalyzes the method for coupling carbon dioxide and epoxide to prepare cyclic carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation of embodiment 1 quaternary phosphonium type deep eutectic ionic liquid

[0025] Benzyltriphenylphosphonium bromide (BTPC) and N-hydroxysuccinimide (NHS) were added to a single-necked flask at a molar ratio of 1:2, and heated under magnetic stirring at 50°C for 0.5 hours , prepared to obtain BTPC-NHS.

[0026] Allyltriphenylphosphonium bromide (ATPB) and N-hydroxysuccinimide (NHS) were added to a single-necked flask at a molar ratio of 1:2, and heated under magnetic stirring at 50°C for 0.5 Hours, prepared to obtain ATPB-NHS.

[0027] Add methyltriphenylphosphonium bromide (MTPB) and N-hydroxysuccinimide (NHS) into single-necked flasks at a molar ratio of 1:2, and heat and magnetically stir at 50°C for 0.5 hours , prepared to obtain MTPB-NHS.

[0028] Tetrabutylphosphonium bromide (TBPB) and N-hydroxysuccinimide (NHS) were added to a single-necked flask at a molar ratio of 1:2, heated and magnetically stirred at 50°C for 0.5 hours to prepare And obtai...

Embodiment 2

[0030]Get the catalyst ATPB-NHS prepared in Example 1 and the reactant propylene oxide and add 25mL of stainless steel autoclave with polytetrafluoroethylene lining successively, wherein, propylene oxide 34.5mmol, ATPB-NHS 2.1 mmol, catalyst accounts for epoxy The molar content of propane is 6mol%; CO is slowly fed into the reactor by controlling the inlet and outlet gas valves 2 Gas to get rid of the residual air inside; after that, close the reactor and heat the reactor oil bath to 60°C, and introduce CO 2 The gas pressure was kept constant to 1.0MPa, and the reaction was continued for 2 hours; after the reaction, the reaction kettle was cooled to room temperature in an ice-water bath, and the product was quantitatively analyzed by gas chromatography. The yield of propylene carbonate was 96%, and the selectivity was ≥99%.

Embodiment 3

[0032] Get the catalyst TBPB-NHS prepared in Example 1 and the reactant epichlorohydrin and add 100mL successively to connect CO 2 The Schlenk (Schlenk) reaction flask of balloon, wherein, epichlorohydrin 10mmol, TBPB-NHS 0.8mmol, catalyst accounts for epichlorohydrin molar content and is 8mol%, decompression gets rid of the air remaining inside; Reaction flask and CO 2 Balloon connected, at a reaction temperature of 25°C, 0.1MPa CO 2 Under pressure conditions, the reaction is continued for 24 hours; after the reaction, the product is quantitatively analyzed by gas chromatography, and the corresponding product yield is 98%, and the selectivity is ≥99%.

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Abstract

The invention relates to a method for preparing cyclic carbonate by coupling carbon dioxide and epoxide with catalyzed quaternary phosphonium type eutectic ionic liquid. The method uses carbon dioxide and different substituent epoxides as raw materials, and uses quaternary phosphonium bromide, N The new deep eutectic ionic liquid synthesized by hydroxysuccinimide according to the molar ratio of 1:2 is used as the catalyst, the catalyst dosage is 2%~8% of the molar weight of the epoxide, the reaction pressure is 0.1~1 MPa, and the reaction temperature is 25 The corresponding cyclic carbonates were synthesized at ~60°C and the reaction time was 2-24 hours. The quaternary phosphonium type deep eutectic ionic liquid adopted in the method is simple to prepare, the raw materials are cheap and easy to obtain, and has excellent catalytic performance, and can catalyze the cyclic carbonate with high selectivity under normal temperature and pressure, metal-free, solvent-free, and co-catalyst-free conditions Synthesis. In addition, the catalyst is easy to separate from the product, has good recycling performance, and is a new environment-friendly catalyst.

Description

technical field [0001] The invention relates to a method for preparing a cyclic carbonate by coupling a quaternary phosphonium type eutectic ionic liquid to catalyze carbon dioxide and an epoxide, and belongs to the field of environment-friendly catalysis. Background technique [0002] carbon dioxide (CO 2 ) is one of the most important greenhouse gases on the earth, and it is also a special renewable C1 resource in my country. It has the advantages of abundant reserves, low price, and non-toxicity. ) is gradually consumed, CO in the atmosphere 2 The concentration increases year by year, causing serious impact on global climate change and ecological environment. Therefore, CO 2 Emission reduction and resource utilization have practical significance for alleviating the greenhouse effect and improving the ecological environment, and are important strategic means to replace fossil fuels and solve the carbon source crisis. However, due to CO 2 It has thermodynamic stability ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36C07D317/46B01J31/02
CPCB01J31/0288B01J31/0298B01J2231/324C07D317/36C07D317/46
Inventor 刘猛帅刘福胜顾永强赵鹏辉王雨辰平冉
Owner QINGDAO UNIV OF SCI & TECH
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