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Pyrazole strongly acidic ionic liquid catalyst and application thereof

An ionic liquid and strong acidic technology, which is applied in the direction of physical/chemical process catalyst, fatty acid esterification, organic compound/hydride/coordination complex catalyst, etc. Cost and other issues, to achieve the effect of shortening the reaction time, reducing the application cost, and increasing the acid density

Inactive Publication Date: 2014-07-30
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are currently many patents and papers on the preparation of biodiesel by acidic ionic liquid catalysis, the acidic ionic liquid involved is relatively small in acidic groups, and the acidity of the ionic liquid is limited, so that a relatively large amount of ionic liquid needs to be added in the catalytic reaction process, and then Increased cost restricts its large-scale application in industrialization

Method used

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  • Pyrazole strongly acidic ionic liquid catalyst and application thereof
  • Pyrazole strongly acidic ionic liquid catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: This pyrazole strongly acidic ionic liquid catalyst is bispyrazole butane sulfonic acid ionic liquid catalyst, and its chemical structural formula is as follows:

[0027] where X is HSO 4 - , m=4; n=4.

[0028] The synthetic method of this ionic liquid catalyst is as follows:

[0029] 1) Dissolve 0.55mol pyrazole and 0.5mol sodium hydroxide in 50ml ethanol solvent, stir and react at 70°C for 10h, cool and filter, wash the filter residue three times with ether (50ml×3), and dry it in a vacuum oven at 50°C for 5h to obtain pyrazole Sodium azole intermediate.

[0030] 2) Dissolve 0.5 mol sodium pyrazole and 0.25 mol 1,4-dibromobutane in 50 ml ethanol, mix well, stir and reflux for 10 h, filter, wash the filtrate three times with ether, and vacuum dry to obtain bispyrazole intermediate.

[0031] 3) 0.5 mol of 1,4-butane sultone was added to the toluene solution of bispyrazole, mixed and stirred for 8 hours, and the toluene was removed by rotary evaporati...

Embodiment 2

[0034] Embodiment 2: this pyrazole strong acid ionic liquid catalyst is dihydrogen phosphate bispyrazole butane sulfonic acid ionic liquid catalyst, and chemical structural formula is as follows:

[0035] where X is H 2 PO 4 - , m=3; n=4.

[0036] The synthetic method of this ionic liquid catalyst is as follows:

[0037] 1) Dissolve 0.55mol pyrazole and 0.5mol sodium hydroxide in 50ml ethanol solvent, stir and react at 70°C for 10h, cool and filter, wash the filter residue three times with ether (50ml×3), and dry it in a vacuum oven at 50°C for 5h to obtain pyrazole Sodium azole intermediate.

[0038] 2) Dissolve 0.5mol sodium pyrazole and 0.25mol 1,3-dibromopropane in 50ml ethanol, mix well, stir and reflux for 10h, filter, wash the filtrate three times with ether, and vacuum dry to obtain bispyrazole intermediate.

[0039] 3) 0.5 mol of 1,4-butane sultone was added to the toluene solution of bispyrazole, mixed and stirred for 8 hours, and the toluene was removed by rota...

Embodiment 3

[0042] Embodiment 3: this pyrazole strongly acidic ionic liquid catalyst is bispyrazole propane sulfonic acid ionic liquid catalyst, and the chemical structural formula is as follows:

[0043] , where X is Cl - , m=4; n=3.

[0044] The synthetic method of this ionic liquid catalyst is as follows:

[0045] 1) Dissolve 0.55mol pyrazole and 0.5mol sodium hydroxide in 50ml ethanol solvent, stir and react at 70°C for 10h, cool and filter, wash the filter residue three times with ether (50ml×3), and dry it in a vacuum oven at 50°C for 5h to obtain pyrazole Sodium azole intermediate.

[0046] 2) Dissolve 0.5 mol sodium pyrazole and 0.25 mol 1,4-dibromobutane in 50 ml ethanol, mix well, stir and reflux for 10 h, filter, wash the filtrate three times with ether, and vacuum dry to obtain bispyrazole intermediate.

[0047] 3) 0.5 mol of 1,3-propane sultone was added to the toluene solution of bispyrazole, mixed and stirred for 8 hours, and the toluene was removed by rotary evaporat...

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Abstract

The invention discloses a pyrazole-based strong acidic ionic liquid catalyst. The catalyst is a pyrazole-based dicationic strong acid ionic liquid. The ionic liquid catalyst has the characteristics of high acid density, high catalytic activity, good stability, short catalytic reaction time, and It has the advantages of mild conditions, simple process, recyclable catalyst and low loss during use. The catalyst in the present invention can be used to prepare biodiesel, and the preparation reaction speed is fast, the reaction time is greatly shortened, and the reaction conditions are mild.

Description

technical field [0001] The invention relates to a pyrazole strongly acidic ionic liquid catalyst and its application, belonging to the technical field of green and renewable energy. Background technique [0002] With the rapid development of the world economy, the demand for energy in various countries has increased sharply, and fossil fuels, as the main energy used by human beings, have been extensively exploited and utilized, which not only brings serious environmental pollution problems, but also has limited reserves. The future development of mankind and the inheritance of human civilization pose a severe test. Therefore, it is imminent to seek renewable energy and resources to replace the gradually depleted fossil fuels. Biodiesel is a long-chain fatty acid methyl ester produced by the transesterification reaction of animal and vegetable oil and methanol. It has the characteristics of easy biodegradation, high cetane number, safe storage and transportation, high energy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C11C3/10
CPCY02E50/13Y02E50/10
Inventor 瞿广飞张军宁平施玉琨
Owner KUNMING UNIV OF SCI & TECH
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