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One-step preparation method for tetrahydrofuran by gas phase hydrogenating maleic anhydride on Cu-Zn-Ti-Ge and using n-butylalcohol as solvent

A technology of tetrahydrofuran and n-butanol, applied in organic chemistry and other fields

Inactive Publication Date: 2010-12-08
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction route of this method is relatively long

Method used

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  • One-step preparation method for tetrahydrofuran by gas phase hydrogenating maleic anhydride on Cu-Zn-Ti-Ge and using n-butylalcohol as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Use 1mol / L HCl solution to TiCl 4 (purity > 98%) was diluted to obtain 1.09mol / LTiCl 4 Diluent. Accurate measurement of TiCl 4 Diluent 22.95ml, Cu(NO 3 ) 2 ·3H 2 O 12.1g, Zn(NO 3 ) 2 ·6H 2 O 29.7g, Ce(NO3) 3 ·6H 2 O 0.4g was dissolved in it to make a mixed solution. Using two constant flow pumps, mix the mixed solution with saturated NaCO 3 The solution was poured into a 1000ml beaker in parallel, heated in a water bath, and the temperature of the water bath was maintained at about 80°C. Stir vigorously while adjusting the flow rate of the constant flow pump to keep the pH of the reaction solution between 8.3. After the precipitation is complete, wash with distilled water, decant, and suction filter repeatedly until the conductivity of the filtrate no longer changes. The sample of about 0.03ms is dried at 120°C for 12h, and then roasted at 350°C for 4h. The samples were pressed into tablets and sieved to make 20-40 mesh granules for later use.

[0023] A f...

Embodiment 2

[0025] Use 1mol / L HCl solution to TiCl 4 (purity > 98%) was diluted to obtain 1.09mol / LTiCl 4 Diluent. Accurate measurement of TiCl 4 Diluent 45.9ml, Cu(NO 3 ) 2 ·3H 2 O12.1g, Zn(NO 3 ) 2 ·6H 2 O 29.7g and Ce(NO3) 3 ·6H 2 O 0.4g was dissolved in it to make a mixed solution. Using two constant flow pumps, mix the mixed solution with saturated NaCO 3 The solution was poured into a 1000ml beaker in parallel, heated in a water bath, and the temperature of the water bath was maintained at about 75°C. Stir vigorously while adjusting the flow rate of the constant flow pump to keep the pH of the reaction solution between 8.3. After the precipitation is complete, wash with distilled water, decant, and suction filter repeatedly until the conductivity of the filtrate no longer changes. The sample of about 0.03ms is dried at 110°C for 12h, and then roasted at 400°C for 2h. The samples were pressed into tablets and sieved to make 20-40 mesh granules for later use.

[0026] Th...

Embodiment 3

[0028] Use 1mol / L HCl solution to TiCl 4 (purity > 98%) was diluted to obtain 1.09mol / LTiCl 4 Diluent. Accurate measurement of TiCl 4 Diluent 45.9ml, Cu(NO 3 ) 2 ·3H 2 O 24.2g, Zn(NO 3 ) 2 ·6H 2 O 29.7g and Ce(NO3) 2 ·6H 2 O 0.4g was dissolved in it to make a mixed solution. Using two constant flow pumps, mix the mixed solution with saturated NaCO 3 The solution was poured into a 1000ml beaker in parallel, heated in a water bath, and the temperature of the water bath was maintained at about 70°C. Stir vigorously while adjusting the flow rate of the constant flow pump to keep the pH of the reaction solution between 8.3. After the precipitation is complete, wash with distilled water, decant, and suction filter repeatedly until the conductivity of the filtrate no longer changes. The sample of about 0.03ms is dried at 120°C for 15h, and then roasted at 350°C for 3h. The samples were pressed into tablets and sieved to make 20-40 mesh granules for later use.

[0029] T...

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Abstract

The invention relates to a method for preparing tetrahydrofuran. Normal butyl alcohol is taken as maleic anhydride solvent, Cu-Zn-Ti-Ce series catalyst maleic anhydride is adopted to prepare the tetrahydrofuran through a singlestage gas phase hydrogenation process, catalyst has the following general formula: Cu<ZnTi><Ce><0.01><O><X>, wherein, a is equal to 0.5-1, b is equal to 0.25-1, and aand b respectively express atomicity of Cu and Ti. X is the oxygen atomicity which is required so as to meet the chemical valence requirement of other elements. The catalyst is prepared by a coprecipitation method. When the normal butyl alcohol is taken as the maleic anhydride solvent, the catalyst is adopted to operate the maleic anhydride gas phase hydrogenation, the higher tetrahydrofuran yield rate can be obtained for a singlestep, at the same time, the normal butyl alcohol generates hydrogen gas, butyl butyrate and butyl aldehyde under the action of the catalyst. The hydrogen gas deprived by the normal butyl alcohol can be used as the raw material to operate the maleic anhydride hydrogenation.

Description

technical field [0001] The invention relates to a method for preparing tetrahydrofuran, in particular to preparing tetrahydrofuran by using n-butanol as a maleic anhydride solvent and adopting a Cu-Zn-Ti-Ce catalyst to hydrogenate maleic anhydride in one step in gas phase. Background technique [0002] Tetrahydrofuran is an excellent low-boiling point (66°C) solvent that can dissolve all polymers except polyethylene, polypropylene, and fluororesin, and is especially suitable for PVC, polyvinylidene fluoride resin, and butylaniline. At the same time, it can be used as an intermediate to produce polyurethane elastomer, spandex elastic fiber, etc. [0003] The industrial production of tetrahydrofuran includes various industrial production methods such as furfural method, 1,4-butanediol catalytic dehydration and cyclization method, butadiene chlorination method and butadiene acetoxylation method. In recent years, a maleic anhydride catalytic hydrogenation method with obvious e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/08B01J23/83
Inventor 殷恒波张瑞超沈玉堂姜廷顺
Owner JIANGSU UNIV