Cross-linked quaternary phosphonium ionic liquid and preparation thereof and application in CO2 cycloaddition reaction
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An ionic liquid and quaternary phosphonium salt technology, applied in the field of industrial catalysis, can solve problems such as being unsuitable for industrial production, and achieve the effects of being suitable for large-scale production, low cost, high selectivity and conversion rate
Inactive Publication Date: 2009-12-30
NORTHWEST NORMAL UNIVERSITY
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However, after the ionic liquid is used as a catalyst to complete the catalytic reaction, vacuum distillation is required to separate the product from the ionic liquid, which is not suitable for industrial production in terms of energy consumption.
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Embodiment 1
[0034] Embodiment 1, preparation of crosslinked quaternary phosphonium salt ionic liquid catalyst
[0035] 1. Raw materials
[0036] Triphenylphosphine is chemically pure, purchased from Sinopharm Chemical Reagent Co., Ltd.;
[0037] 4-vinylbenzyl chloride was purchased from Alfa Aesar;
[0038] Ethylene glycol dimethacrylate was purchased from Shanghai Jingchun Reagent Co., Ltd.;
[0039] Azobisisobutyronitrile is analytically pure.
[0040] Neptone and tetrahydrofuran were of analytical grade, purchased from Sinopharm Chemical Reagent Co., Ltd., and used directly without treatment.
[0041] 2. Process
[0042] (1) Synthesis of quaternary phosphonium salt ionic liquid
[0043] Mix 0.1 mol of 4-vinylbenzyl chloride and 0.1 mol of triphenylphosphine, heat to 50°C, and react for 24 hours to obtain a quaternary phosphine salt ionic liquid. Yield: 82%.
[0044] (2) Preparation of crosslinked quaternary phosphonium salt ionic liquid
[0045] Mix 1g of ethylene glycol dimeth...
Embodiment 2
[0053] Example 2. Application of cross-linked quaternary phosphonium salt ionic liquid in carbon dioxide cycloaddition reaction
[0054] Add 3mL of epichlorohydrin, a magneton, and 0.1g of the catalyst prepared in this paper into a 100mL stainless steel autoclave, and place it at 160°C and a pressure of 5Mpa after replacing the air. The reaction was stirred for 2 hours. After the reaction is over, cool down, release gas, and filter the mixture to obtain the corresponding cyclic carbonate. The yield reached 99.2%. Its selectivity is 100%.
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Abstract
The invention provides a cross-linked quaternary phosphonium ionic liquid. The preparation method comprises the following steps: mixing 4-ethenyl benzyl chloride with triphenyl phosphonium at mol ratio of 1:1-1:1.5, heating to the room temperature to 60 DEG C, and reacting for 20-48h to obtain the quaternary phosphonium ionic liquid; mixing ethylene glycol dimethacrylate with the quaternary phosphonium ionic liquid at mol ratio of 1:1-5:1, adding azo diisobutyronitrile which is 1-5% of the total molar weight of the ethylene glycol dimethacrylate and the quaternary phosphonium ionic liquid, heating to the temperature of 60-90 DEG C, and reacting for 20-48h; and washing reaction products by acetone and tetrahydrofuran in turn to obtain the cross-linked quaternary phosphonium ionic liquid. Experiment proves that the cross-linked quaternary phosphonium ionic liquid catalyst provides high catalytic activity to a reaction of CO2 epoxy compound for generating five-membered cycle compound, and has very high selectivity and high conversion rate. Reaction conditions are optimized, yield is up to 99.2%, and the selectivity is 100%.
Description
technical field [0001] The invention belongs to the technical field of industrial catalysis and relates to a CO 2 Catalysts for cycloaddition reactions, especially involving a novel CO with high selectivity and high conversion 2 Cycloaddition reaction nano-catalyst - cross-linked quaternary phosphonium salt ionic liquid; the present invention also relates to the preparation method of the nano-catalyst and the CO 2 Applications in cycloaddition reactions. Background technique [0002] CO 2 It is the final oxidation product of carbon-containing compounds, and its massive discharge not only wastes resources, but also pollutes the environment and causes a global greenhouse effect. CO 2 It has the advantages of safety and cheapness, and it can be used reasonably and effectively as a rich carbon resource, which is of great significance in terms of economic and social benefits. [0003] Currently, development is based on CO 2 Fixed green chemistry has been widely concerned by...
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