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Process for catalyzing synthesizing tetrahydrofuran by granule type solid super strengthen acid

A solid superacid and tetrahydrofuran technology, applied in the direction of organic chemistry, can solve the problems of catalyst and reaction system separation, corrosion, production process changes, etc., and achieve the effect of excellent catalytic activity, simple process and single raw material

Inactive Publication Date: 2006-06-28
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process is usually catalyzed by sulfuric acid, which corrodes equipment, causes serious coking, and easily causes environmental pollution.
Adopt strongly acidic ion exchange resin (Zhu Chongye, Chen Zhumin, Li Quanzhi, petrochemical industry, the 19th volume 518 in 1990) and η-Al 2 o 3 , heteropoly acid, etc. instead of sulfuric acid catalysis, effectively solved the problem of equipment corrosion and coking, and reduced environmental pollution, but the production process has not changed much, and there is still the problem of separation of catalyst and reaction system
x-Al 2 o 3 Or H-Y molecular sieve fixed bed (Wang Haijing, Duan Qiwei, Chemical Industry Progress, 2002, Volume 21, No. 12, Page 934) catalytic synthesis of THF has the advantages of high catalytic efficiency, continuous production, and no need for separation of catalysts, but the catalytic temperature is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add catalyst: In the reactor, add 3-5mm granular SO 4 2- / Al 2 o 3 Solid superacid catalyst 80g.

[0025] (2) Heating with the electric heating wire under the control of the controller; heating to make the temperature reach 250°C;

[0026] (3) Feed nitrogen: import nitrogen into the reactor with a space velocity of 60ml / h, and make the catalyst in the nitrogen protection state all the time;

[0027] (4) input 1.4-butanediol: after the air in the reaction system was evacuated, import 1.4-butanediol vapor in the reactor with a weight space velocity of 25g / h;

[0028] (5) product generation: 1.4-butanediol generates product under the action of catalyst;

[0029] (6) Product post-treatment: after the above reaction, the product aqueous solution sent out from the reactor discharge port is condensed by a condensing device and collected in a flask.

[0030] (7) Split flow purification: the above crude product is split, and the 64-67C fraction is collected to obtain a...

Embodiment 2

[0033] (1) Add catalyst: In the reactor, add 3-5mm granular SO 4 2- / MxOy solid superacid catalyst 100g.

[0034] (2) Only use the electric heating wire under the control of the controller to heat; heating makes the temperature rise to 280°C

[0035] (3) Feed nitrogen: import nitrogen into the reactor with a space velocity of 80ml / h, and make the catalyst in the nitrogen protection state all the time;

[0036] (4) input 1.4-butanediol: after the air in the reaction system was evacuated, import 1.4-butanediol vapor in the reactor with a weight space velocity of 30g / h;

[0037] (5) product generation: 1.4-butanediol generates product under the action of catalyst;

[0038] (6) Product post-treatment: after the above reaction, the product aqueous solution sent out from the reactor discharge port is condensed by a condensing device and collected in a flask.

[0039] (7) Split flow purification: split the above crude product, collect fractions at 64-67° C., and obtain a crude pr...

Embodiment 3

[0041] (1) Add catalyst: In the reactor, add 3-5mm granular SO 4 2- / MxOy solid superacid catalyst 120g;

[0042] (2) Heating with the electric heating wire under the control of the controller; heating to make the temperature rise to 300°C

[0043] (3) Feed nitrogen: import nitrogen into the reactor with a space velocity of 70ml / h, and make the catalyst in the nitrogen protection state all the time;

[0044] (4) input 1.4-butanediol: after the air in the reaction system was evacuated, import 1.4-butanediol vapor in the reactor with a weight space velocity of 35g / h;

[0045] (5) product generation: 1.4-butanediol generates product under the action of catalyst;

[0046] (6) Product post-treatment: after the above reaction, the product aqueous solution sent out from the reactor discharge port is condensed by a condensing device and collected in a flask.

[0047] (7) Split flow purification: split the above crude product, collect fractions at 64-67° C., and obtain a crude prod...

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PUM

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Abstract

The invention discloses a method to compound tetrahydrofuran catalyzed by particle solid super strong acid that includes the steps of adding catalyst, heating, adding nitrogen gas, adding 1,4-butanediol butylene glycol, compounding result, post processing, fractionation and purifying. The invention has advantages of high catalyzing efficiency, low reaction temperature, single raw material, high yield, low cost, etc.

Description

technical field [0001] The invention relates to a catalytic synthesis method of an organic solvent, in particular to a method for catalytic synthesis of tetrahydrofuran by using a solid superacid. Background technique [0002] Tetrahydrofuran (THF) is a highly polar, low-boiling amphoteric solvent commonly used in organic research and industry, and is also an important intermediate for drug synthesis and organic chemical raw materials. In the pharmaceutical industry, tetrahydrofuran is used as a solvent for the synthesis of Kebiqing, Lifuzyme, progesterone and some hormonal drugs; tetrahydrofuran can also be used for the synthesis of leather surface treatment agents, and paper chromatography of amino peptides. [0003] At present, the main methods for synthesizing THF are: furfural method, dichlorobutene method, maleic anhydride catalytic hydrogenation method, Reppe, butadiene oxidation method and 1,4-butanediol dehydration and cyclization method. In the above method, the T...

Claims

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Application Information

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IPC IPC(8): C07D307/08
Inventor 高根之李谚信郑晓凤
Owner QUFU NORMAL UNIV
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