A one-pot high-yield producing method for tetrahydrothiophene

A tetrahydrothiophene, high-yield technology, applied in the direction of organic chemistry, can solve the problems of difficult product separation, affecting the application of downstream products, and difficult separation of water and products, achieving high yield and purity, low cost, and environmental pollution small effect

Active Publication Date: 2017-02-15
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that water is generated during the reaction process, which brings certain difficulties to product separation and directly affects the application of downstream products.
The process has the characteristics of low raw mat...

Method used

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  • A one-pot high-yield producing method for tetrahydrothiophene
  • A one-pot high-yield producing method for tetrahydrothiophene
  • A one-pot high-yield producing method for tetrahydrothiophene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Past figure 1 Add 164Kg60% content of anhydrous sodium sulfide in the shown 1000 liters of enamel reaction kettle 1, 480Kg solvent N-methylpyrrolidone, 3.2Kg phase transfer catalyst benzyltriethylammonium chloride, stir and heat up; keep the reaction temperature at 50-100°C , Slowly add 160Kg of 1,4-dichlorobutane into the reactor 1 dropwise. After the dropwise addition is completed, the reaction time is 3 to 6 hours. Continue heating to 115-122°C, and use the enamel packed tower 2 to distill under normal pressure to obtain the refined tetrahydrothiophene. The tetrahydrothiophene fine product weighs 142.5Kg, the tetrahydrothiophene content is 99% according to gas chromatography analysis, and the yield is greater than 95%. The tail gas is cooled by the sheet-type enamel condenser 3, separated by the gas-liquid separator 4, and enters the tail gas absorption tank 5 to be absorbed by water and alkali, and then emptied.

Embodiment 2

[0021] Embodiment 2~6: with embodiment 1, only anhydrous sodium sulfide consumption is different.

[0022] During the reaction process, keep 480Kg N-methylpyrrolidone, 160Kg 1,4-dichlorobutane, 3.2Kg phase transfer catalyst benzyltriethylammonium chloride, the reaction temperature is 50-100°C, and the reaction time is 3-6 hours , by changing the amount of anhydrous sodium sulfide, investigate the effect of the amount of anhydrous sodium sulfide on the yield of tetrahydrothiophene.

[0023] According to the content of tetrahydrothiophene detected by gas chromatography, the yield of calculated tetrahydrothiophene is shown in Table 1.

[0024] The impact of the amount of anhydrous sodium sulfide in table 1 on the yield of tetrahydrothiophene

[0025]

[0026] As can be seen from Table 1, in the case of 160Kg 1,4-dichlorobutane, changing the addition of anhydrous sodium sulfide, the addition of anhydrous sodium sulfide is 164 ~ 205Kg can meet the production needs. It shows th...

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Abstract

The invention relates to a one-pot high-yield producing method for tetrahydrothiophene. The method includes adding 164-205 kg of anhydrous sodium sulfide having a content of 60%, 480-800 kg of a solvent and 3.2-9.6 kg of a phase transfer catalyst into an enamel reactor having a volume of 1500 L, heating under stirring, maintaining the reaction temperature to be 50-100 DEG C, adding dropwise 160 kg of 1,4-dichlorobutane into the reactor, maintaining the temperature for 3-6 h after the addition is finished, heating to 115-122 DEG C, and performing atmospheric distillation by adopting an enamel filler column to obtain a tetrahydrothiophene high-quality product. The purity of the product of the method can be 99%, and the yield is higher than 95%. The method is high in product yield and purity, low in environment pollution, low in cost and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for producing tetrahydrothiophene with high yield in one pot. Background technique [0002] Tetrahydrothiophene is an important sulfur-containing saturated heterocyclic compound. It is a colorless or slightly yellow transparent liquid. It has stable chemical properties, is not easily oxidized by air, has unique taste, is safe and efficient, and is mainly used as an odorant for gas and natural gas. It is widely used at home and abroad, and can also be used as a natural gas odor enhancer, chain transfer inhibitor, modifier and catalyst. In addition, tetrahydrothiophene can also be used to synthesize a variety of intermediates for new medicines, pesticides and polymer synthetic material additives. With the advancement of science and technology, many new application fields have been continuously developed, and the potential demand at home and abroad is very large. [0003] The synthetic method of existing tetrahydrothiop...

Claims

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Application Information

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IPC IPC(8): C07D333/08
CPCC07D333/08
Inventor 徐保明赖晓玲时爽许庆博徐思思陈坤唐强胡传群
Owner HUBEI UNIV OF TECH
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