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Method of preparing tetrahydrofuran

A technology of tetrahydrofuran and butanediol, applied in chemical instruments and methods, organic chemistry, physical/chemical process catalysts, etc., can solve the problems of low tetrahydrofuran yield, dangerous methods, etc., and achieve the effect of excellent reactivity

Inactive Publication Date: 2008-08-20
HYOSUNG CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of low yield and dangerous method for preparing tetrahydrofuran, an object of the present invention is to provide a safer and more convenient method for preparing tetrahydrofuran

Method used

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  • Method of preparing tetrahydrofuran

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Embodiment 1

[0025] A fixed bed reactor with a diameter of 20 mm and a length of 520 mm was used for the gas phase catalytic reaction. First, 2 g of aluminum sulfate catalyst was charged into the reactor, and the catalyst was activated with helium at 370° C. for 2 hours. Using a syringe pump, 1,4-butanediol at a flow rate of 0.5 cc / min was mixed with helium and fed into the reactor at a constant flow rate of 5.0 liters / hour. The reaction was carried out at 200° C. under one atmospheric pressure, and the reaction products were analyzed on-line using a Poropak QS column and a gas chromatograph equipped with a flame ionization detector (FID). After the reaction reached a steady state, the products passing through the reactor were analyzed. The yield of tetrahydrofuran was 98.5%.

Embodiment 2

[0027] The liquid-phase catalytic reaction was carried out in a 500 ml three-necked round bottom reactor equipped with a magnetic stirrer and reflux device. Before the reaction, the catalyst was activated with helium gas at 300° C. for 2 hours, and 0.5 g of pretreated aluminum sulfate and 100 g of 1,4-butanediol were added to the reactor. The reaction was carried out at a temperature of 200° C. for 1 hour, and the reaction product was condensed using a condenser. The condensed product was then distilled to separate residual 1,4-butanediol and analyzed using a gas chromatograph as described in Example 1. As a result, 98.5% tetrahydrofuran was obtained.

Embodiment 3-5

[0029] Except using one of transition metal sulfate catalysts such as nickel sulfate, ferrous sulfate and chromium sulfate of 1g and 100g of 1,4-butanediol respectively, all the other are in the same manner as described in Example 2 The preparation process of tetrahydrofuran was carried out. The yields for each reaction are listed in Table 1.

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Abstract

The present invention relates to a process for preparing tetrahydrofuran from 1,4-butandiol. According to the process in the present invention, a metal sulfate catalyst selected from the group consisting of aluminum sulfate, nickel sulfate, ferrous sulfate and chrome sulfate is pre-treated with an inert gas to be activated, followed by introducing into a reactor together with 1,4-butandiol.

Description

technical field [0001] The present invention relates to a method for preparing tetrahydrofuran from 1,4-butanediol in the presence of a metal sulfate catalyst. [0002] Tetrahydrofuran is widely used as a solvent for organic compounds or a synthetic raw material for polymers in various fields. Recently, it has been used more and more as a raw material and additive for various polymers. [0003] Tetrahydrofuran can be prepared in a number of ways. According to the prior art, tetrahydrofuran is generally prepared by dehydration of 1,4-butanediol or hydrogenation of furan. In the method for producing tetrahydrofuran based on the dehydration of 1,4-butanediol, 1,4-butanediol is reacted in the presence of an acidic catalyst, and then water is separated and removed from the obtained tetrahydrofuran. The efficiency of the method for preparing tetrahydrofuran depends on the performance of the acid catalyst used in the reaction, so it is more important to develop an efficient cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/08B01J27/053
CPCC07D307/08
Inventor 李垠九白龙浩
Owner HYOSUNG CORP