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Production method of tetrahydrofuran

A technology of tetrahydrofuran and its production method, which is applied in the field of preparation of tetrahydrofuran, can solve problems such as not mentioned, and achieve the effects of prolonging service life, suppressing side reactions, and reducing investment and operating costs

Active Publication Date: 2015-06-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, in the above-mentioned disclosed patents, there is no mention of the impact of the properties of the 1,4-butanediol raw material on the dehydration cyclization reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A fixed-bed isothermal reactor is used to mix the raw materials composed of 1,4-butanediol 99.52%, 2-(4-hydroxybutoxy)tetrahydrofuran 0.48% and hydrogen continuously through the palladium resin catalyst, the palladium content of the catalyst used 0.05%, the commercially available brand of resin is D005 type macroporous cation exchange resin. Control the reaction temperature at 100°C, the reaction pressure at 0.6MPa, the molar ratio of hydrogen to alcohol at 10, and the liquid hourly space velocity of 1,4-butanediol at 1.5h -1 , The liquid phase product was collected after the reaction product was cryogenically cooled, and its composition was analyzed by gas chromatography. Run continuously for 500 hours under this condition, and the reaction conditions and reaction results are shown in Table 1.

Embodiment 2

[0032] A fixed-bed isothermal reactor is used to mix the raw materials consisting of 99.52% of 1,4-butanediol and 0.48% of 2-(4-hydroxybutoxy)tetrahydrofuran with hydrogen and then continuously pass through the palladium resin. The palladium content of the catalyst used is 0.05% %, the commercially available brand of resin is D005 type macroporous cation exchange resin. Control the reaction temperature at 100°C, the reaction pressure at 0.2MPa, the molar ratio of hydrogen to alcohol at 6, and the liquid hourly space velocity of 1,4-butanediol at 1.0h -1 , The liquid phase product was collected after the reaction product was cryogenically cooled, and its composition was analyzed by gas chromatography. Run continuously for 500 hours under this condition, and the reaction conditions and reaction results are shown in Table 1.

Embodiment 3

[0034] A fixed-bed isothermal reactor is used to mix the raw materials consisting of 99.22% of 1,4-butanediol and 0.78% of 2-(4-hydroxybutoxy)tetrahydrofuran with hydrogen and then continuously pass through the palladium resin catalyst. The palladium content of the catalyst used 0.07%, the commercially available brand of resin is D72 type macroporous cation exchange resin. Control the reaction temperature at 100°C, the reaction pressure at 0.6MPa, the molar ratio of hydrogen to alcohol at 10, and the liquid hourly space velocity of 1,4-butanediol at 1.5h -1 , The liquid phase product was collected after the reaction product was cryogenically cooled, and its composition was analyzed by gas chromatography. Run continuously for 500 hours under this condition, and the reaction conditions and reaction results are shown in Table 1.

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Abstract

The invention discloses a production method of tetrahydrofuran. The tetrahydrofuran is produced from coarse 1,4-butanediol containing 2-(4'-hydroxybutoxyl) tetrahydrofuran through continuously cyclodehydrating under the action of a palladium-supported sulfonated ion exchange resin catalyst in the presence of hydrogen. The palladium-supported sulfonated ion exchange resin catalyst generally contains 0.02-1.50% of palladium, the cyclodehydration is generally carried out under the reaction conditions that the hydrogen and the raw material (100% of 1,4-butanediol) are in the molar ratio of 1-100, the reaction temperature is 50-170 DEG C, the reaction pressure is 0.02-2.0MPa, and the liquid hour (volume) space velocity of 1,4-butanediol is 0.5-5.0h<-1>. According to the method, 1,4-butanediol containing 2-(4'-hydroxybutoxyl) tetrahydrofuran is used as a raw material, the high-selectivity tetrahydrofuran is produced continuously and stably in a long period under the condition of low temperature, and the method is suitable for industrial application.

Description

technical field [0001] The invention relates to a method for preparing tetrahydrofuran, in particular to a method for preparing tetrahydrofuran by dehydrating and cyclizing 1,4-butanediol as a raw material. Background technique [0002] Tetrahydrofuran (THF) is a low-toxic solvent with high polarity, low boiling point and excellent performance. It is widely used as a solvent for surface coatings, anti-corrosion coatings and film coatings. Its main purpose is to produce polytetramethylene ether glycol (PTMEG), polyurethane elastomers and polyurethane artificial leather, etc., are also used as solvents for esterification and polymerization reactions, as well as raw materials for some pharmaceutical intermediates such as hormone drugs. [0003] At present, the production methods of tetrahydrofuran include: furfural hydrogenation method, maleic anhydride direct hydrogenation method and 1,4-butanediol dehydration and cyclization method. Among them, the furfural method has been g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/08
Inventor 陈明苏杰乔凯翟庆铜张宝国张淑梅周峰
Owner CHINA PETROLEUM & CHEM CORP
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