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Method and device for producing thiophene and derivative thereof in direct-cooled mode

A production method and technology for thiophene are applied in the field of production methods and devices implementing the method, and can solve the problems of reactor coking blockage, thiophene loss, and high energy consumption

Active Publication Date: 2010-02-24
LIANYUNGANG DIPU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent application (publication numbers are CN 1335313A and CN 1420116A) discloses the production process and equipment of butadiene-sulfur to synthesize thiophene, the reaction product is only cooled by a circulating water condenser, thiophene is lost in a large amount from the tail gas, and 1 ton of thiophene raw material is produced The consumption of butadiene (unit consumption) former is 1.4 tons (yield 46%), and the latter is 1.8 tons (yield 36%); Heating the reactor is completely unnecessary because the reaction is an exothermic reaction, but because the resistance wire is used to heat the reaction raw materials, the inlet temperature of the reactor is relatively low, and the reactor has to be heated, resulting in high energy consumption , the reactor is coked and blocked; in addition, the reactors of the above two Chinese patent applications are filled with fillers, and no corresponding technical effect has been achieved, which makes the reactor coked and blocked faster

Method used

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  • Method and device for producing thiophene and derivative thereof in direct-cooled mode
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  • Method and device for producing thiophene and derivative thereof in direct-cooled mode

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Experimental program
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Effect test

Embodiment 1

[0073] The production of embodiment 1 thiophene

[0074] The butadiene is pumped from the butadiene metering tank T130 to the butadiene vaporizer E131, and the feed rate is 60Kg / h. The water B is pumped to the water B vaporizer E121, and the feed rate is 5Kg / h. The butadiene and water B coming out of the vaporizer enter the butadiene heating furnace H132 together, and are heated to 250°C to obtain water B-butadiene gas.

[0075] The solid sulfur is poured into the sulfur melting tank T141, pumped to the feed inlet on the top of the sulfur heating furnace E140, and the feed rate is 65Kg / h. The water A is pumped to the water A vaporizer E111, the feed rate is 20Kg / h, and then enters the water heating furnace E112 to be heated to 420°C, and then enters the feed inlet below the sulfur heating furnace E140. Water A and sulfur are heated to 540°C in a sulfur furnace to obtain water A-sulfur gas.

[0076]Water A-sulfur gas and water B-butadiene gas enter the reactor R210 respectiv...

Embodiment 2

[0083] The production of embodiment 2 thiophenes

[0084] Production process and device are with embodiment 1, and its difference is only in:

[0085] The mixing section of the reactor is a φ219×6 stainless steel tube with a length of 0.6 meters; the reaction section is a φ89×6 stainless steel tube with a length of 8 meters. Feed amount butadiene 100Kg / h, sulfur 110Kg / h, water A 35Kg / h, water B 5Kg / h. The reactor inlet temperature is 380°C, the outlet temperature is 450°C, and the pressure is 0.02MPa (gauge pressure). Feed ratio sulfur / butadiene 0.93mol, water / butadiene 1.2mol, reaction residence time 0.92s. The output of thiophene is 1400Kg per day, the unit consumption of butadiene is 1.71 tons, and the yield is 38%. The operation is stopped once every 8 days to clean up the coke in the reactor and the sulfur in the pipeline, and the monthly production of thiophene is 35 tons.

Embodiment 3

[0086] The production of embodiment 3 thiophenes

[0087] Production process and device are with embodiment 1, and its difference is only in:

[0088] The mixing section of the reactor is a φ273×6 tube with a length of 0.8 meters; the reaction section is a φ133×6 stainless steel tube with a length of 8 meters. Feed amount of butadiene 135Kg / h, sulfur 144Kg / h, water A 45Kg / h, water B 10Kg / h. The reactor inlet temperature is 370°C, the outlet temperature is 450°C, and the pressure is 0.02MPa (gauge pressure). Feed ratio sulfur / butadiene 0.9mol, water / butadiene 1.22mol, reaction residence time 1.33s. The output of thiophene is 1750Kg per day, the unit consumption of butadiene is 1.85 tons, and the yield is 35%.

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Abstract

The invention discloses method and device for producing thiophene and a derivative thereof by synthesizing butadiene and sulfur. The production method comprises the steps of reaction, separation and desulfurization. In the reaction process, an intermediate frequency furnace is adopted to heat raw materials to initial reaction temperature; the reaction is carried out in a gas phase under normal pressure at the temperature of 360-460 DEG C; the molar ratio of the sulfur to the butadiene is 0.9-1.5, the molar ratio of water to the butadiene is 0.5-3, and the retention time of the reaction is 0.3-5 seconds. The reaction product is directly cooled by water spraying; thiophene in a gas phase is recovered by vaporizing and cooling the raw material butadiene; then tar generated in the reaction isused for absorbing the thiophene recovered again in a gas phase; and the yield of the thiophene is 40-50 percent. A steam stripping method is firstly used for separating the thiophene from the tar inthe reaction product, and then the steam stripped thiophene is rectified to obtain a finished thiophene product with a purity of 99.6-99.8 percent. The method and the device can be used for producingthiophene derivatives such as 3-methyl thiophene, and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a production method of thiophene and its derivatives and a device for implementing the method. Background technique [0002] Thiophene is the transliterated name of Thiophene in English, and it is also called a thiadiene pentacyclic ring and thiamolo in Chinese. Thiophene is the most important sulfur heterocyclic compound, mainly used in the production of pharmaceutical intermediates, and is also widely used in the synthesis of pesticides, dyes, polymer additives, etc. As an important pharmaceutical raw material, thiophene derivatives synthesized from thiophene are used to synthesize hundreds of drugs such as cephalosporins and cephalosporins. [0003] The earliest production method of thiophene was extraction from the pickling solution of the benzene fraction of coal tar. Meets the requirements of the pharmaceutical industry. This method has long been eliminated and replaced by...

Claims

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Application Information

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IPC IPC(8): C07D333/10C07D333/08C07D333/28B01D53/48B01D53/52B01D53/78B01D53/14
Inventor 杨顺立
Owner LIANYUNGANG DIPU CHEM
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