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A kind of ionic liquid catalyst, its preparation method and application

A technology of ionic liquid and catalyst, which is applied in the field of new catalysts, can solve the problems of low catalyst activity and high catalytic activity, and achieve the effects of high catalytic activity, simple preparation process, high glycerin conversion rate and product yield

Active Publication Date: 2020-05-19
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its purpose is to functionalize the quaternary ammonium salt, and then use it as a cation to screen suitable anions to form an ionic liquid catalyst, obtain high catalytic activity, and reduce its cost to solve the problem of existing glycerin and CO 2 Technical Problems of Low Catalyst Activity for Synthesis of Glycerol Carbonate by Coupling Reaction

Method used

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  • A kind of ionic liquid catalyst, its preparation method and application
  • A kind of ionic liquid catalyst, its preparation method and application
  • A kind of ionic liquid catalyst, its preparation method and application

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preparation example Construction

[0050] When functionalized group FG is amino group, the preparation method of this ionic liquid catalyst comprises the steps:

[0051] (1) Mix trialkylamine and alkylating agent halide ammonium salt according to molar ratio (1~6): 1, preferably 5: 1, and dissolve in absolute ethanol, in N 2 Under protection, reflux reaction is carried out at about the boiling point of ethanol for 12-36 hours, preferably 24 hours, to obtain solution A; the number of carbon atoms in the alkyl group in the trialkylamine is preferably an integer of 1-12, and triethylamine is more preferred. Alkylating agent halide ammonium salt is preferably halide primary ammonium salt, with structural formula X-(CH 2 ) n -NH 2 HX represents, wherein X is a halogen element, preferably I; n is an integer ranging from 1 to 12, and is preferably a haloethylammonium salt.

[0052] (2) Cool solution A obtained in step (1) to room temperature (20-30° C.), filter to remove insoluble matter, and then distill off ethan...

Embodiment 1

[0070] One for glycerol and CO 2 An ionic liquid catalyst for synthesizing glycerol carbonate by a coupled reaction method, the cation of the ionic liquid is a functionalized quaternary ammonium salt ion, and the anion is Cl - , the functionalized group of the functionalized quaternary ammonium salt ion is an amino group. The ionic liquid is named aminoethyltriethylammonium chloride, i.e. Aminoethyl triethylamine Chloride, [AETEA]Cl, and its structural formula is as follows:

[0071]

[0072]

[0073] Described ionic liquid catalyst, its preparation method, comprises the following steps:

[0074] (1) A certain amount of triethylamine and alkylating agent chloroethylamine hydrochloride are added in dehydrated alcohol, in N 2 Under protection, reflux at 75°C for 24 hours to obtain solution A. The ratio of the amount of substances of triethylamine and chloroethylamine hydrochloride is 5:1;

[0075] (2) Solution A obtained in step (1) is cooled to room temperature, and t...

Embodiment 2

[0083] One for glycerol and CO 2 An ionic liquid catalyst for synthesizing glycerol carbonate by a coupled reaction method, the cation of the ionic liquid is a functionalized quaternary ammonium salt ion, and the anion is Br - , the functionalized group of the functionalized quaternary ammonium salt ion is an amino group. The ionic liquid is named aminoethyltriethylammonium bromide, i.e. Aminoethyl triethylamine Bromide, [AETEA]Br, and its structural formula is as follows:

[0084]

[0085] Described ionic liquid catalyst, its preparation method is identical with embodiment 1, but changes alkylating agent to be bromoethylamine hydrobromide.

[0086] Catalyst characterization, as attached figure 2 Shown is the H NMR spectrum characterization result of the ionic liquid catalyst: 1 H NMR (400MHz, CD 3 CN)δ3.56(d,J=7.0Hz,2H),3.27(dd,J=14.5,7.2Hz,6H),3.17–3.08(m,2H),1.27(dd,J=16.5,9.2Hz, 9H), 1.14 (t, J=7.0Hz, 2H).

[0087] Catalyst characterization, as attached image 3...

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Abstract

The invention belongs to the field of novel catalysts, in particular to an ionic liquid catalyst, a preparation method and an application thereof. The invention more particularly relates to an ionic liquid catalyst for synthesizing glycerol carbonic ester by a coupled reaction method of glycerinum and CO2, a preparation method and an application. Anions of the ionic liquid catalyst are functionalquaternary ammonium salt ions, and cations are halide ions or hydroxyl ions; the functional groups of the functional quaternary ammonium salt ions are amino, carboxyl or hydroxyl. The functional quaternary ammonium salt ionic liquid is used for catalyzing coupled reaction method of glycerinum and CO2 to synthesize the glycerol carbonic ester. In the optimum condition, the conversion ratio of glycerinum can reach up to 95%, and the yield of glycerol carbonic ester can reach 89%. The developed ionic liquid catalyst has the advantages of high catalytic activity, simplicity in preparation, low cost and small dosage of the catalyst.

Description

technical field [0001] The invention belongs to the field of novel catalysts, in particular, it relates to an ionic liquid catalyst, its preparation method and application, more specifically, it relates to a catalyst for glycerin and CO 2 An ionic liquid catalyst for synthesizing glycerol carbonate by coupled reaction method, its preparation method and application. Background technique [0002] In recent years, biodiesel has received extensive research and attention due to its renewable, environment-friendly and excellent combustion properties, and the global production of biodiesel has grown rapidly. On the other hand, the industrialization of biodiesel produces a large amount of by-product glycerol. According to reports, for every 1kg of biodiesel produced, 0.1kg of glycerin will be produced by-product. Therefore, it is urgent to realize the efficient conversion of glycerol to promote the sustainable development of biodiesel industrialization. A variety of glycerol conv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07D317/36
CPCB01J31/0279B01J2231/49C07D317/36
Inventor 王华军周雄徐杏
Owner HUAZHONG UNIV OF SCI & TECH