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
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[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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