Method and device for producing thiophene and derivant thereof

A production method and production device technology, which is applied in the field of production methods and devices of thiophene and its derivatives, can solve the problems of heating, sulfur clogged pipes, and cooling to 20°C, etc., to solve the problem of strong odor, sulfur clogging, Achieve cleaning effect

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

However, the above-mentioned Japanese patents have not been industrialized. One of the possible reasons is that the unreacted sulfur of the reaction product clogs the pipes and condensers after cooling; another possible reason is that the recovery of thiophene in the tail gas cannot be solved. A large amount of thiophene is entrained in the by-product gas hydrogen sulfide (tail gas), which cannot be completely cooled by water condenser alone. Even if the tail gas is frozen by other methods, it can only be cooled to 20°C (if it is lower, the freezer will be blocked) , there is still a large amount of thiophene loss
Chinese patent application (publication numbers are CN 1335313A and CN 1420116A) discloses the production process and equipment of butadiene-sulfur synthetic thiophene, and the reaction adopts the method disclosed in the above-mentioned Japanese patent, and the reaction product is only cooled by a circulating water condenser , thiophene is lost in a large amount from the tail gas, and the consumption (unit consumption) of 1 ton of thiophene raw material butadiene is 1.4 tons (yield 46%) for the former, and 1.8 tons (yield 36%) for the latter; meanwhile, the Chinese patent application (publication numbers are CN 1335313A and CN 1420116A) all heat the reactor, because the reaction is an exothermic reaction, so this is completely unnecessary in fact, but because it adopts resistance wire to heat the reaction raw material, the inlet temperature of the reactor is relatively low , had to heat the reactor
But in this way, the working life of the reactor is reduced, the electric heating efficiency is also affected, and the production cost is increased.

Method used

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  • Method and device for producing thiophene and derivant thereof
  • Method and device for producing thiophene and derivant thereof
  • Method and device for producing thiophene and derivant thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] The production of embodiment 1 thiophene

[0086] The butadiene is pumped from the butadiene metering tank T111 to the water heat exchangers E1111 and E1112 with a feed rate of 150Kg / h. After exchanging heat with circulating water, it enters the butadiene vaporizer E112 and is heated to 120°C. The water vapor enters the water B evaporator E114 through the flowmeter, the feed rate is 10Kg / h, and it is heated to 140°C. The butadiene and water B from the vaporizer enter the butadiene heating furnace H113 and are heated to 250°C. The solid sulfur is poured into the sulfur melting tank T121, pumped to the feed inlet of the sulfur heating furnace H123, and the feed rate is 275Kg / h. The water vapor enters the water A vaporizer E131 through the flowmeter, the feed rate is 80Kg / h, and is heated to 140°C, then enters the water heating furnace H132 and is heated to 530°C, and then enters the feeding port below the sulfur heating furnace H123. Water A and sulfur are heated to 540...

Embodiment 2

[0096] The production of embodiment 2 thiophenes

[0097] Process flow and device are with embodiment 1, and its difference is only in:

[0098] Feed amount butadiene 130Kg / h, sulfur 234Kg / h, water A 80Kg / h, water B 10Kg / h. The outlet temperature of the butadiene furnace is 250°C, and the outlet temperature of the sulfur furnace is 545°C. The reactor inlet temperature is 390°C, the outlet temperature is 420°C, the pressure is 0.02MPa (gauge pressure), and the tar kettle outlet temperature is 160°C. Feed ratio sulfur / butadiene 1.52mol, water / butadiene 2.08mol, reaction residence time 1.90s. The output is 2700Kg per day. The unit consumption of butadiene is 1.16 tons, and the yield is 55%. Stop once every 20 days of operation to clean up the tar kettle.

Embodiment 3

[0099] The production of embodiment 3 thiophene

[0100] Process flow and device are with embodiment 1, and its difference is only in:

[0101] Feed amount of butadiene 167Kg / h, sulfur 290Kg / h, water A 90Kg / h, water B 10Kg / h. The outlet temperature of the heating furnace is 250°C for the butadiene furnace and 510°C for the sulfur furnace. The reactor inlet temperature is 375°C, the outlet temperature is 450°C, the pressure is 0.02MPa (gauge pressure), and the tar kettle outlet temperature is 210°C. Feed ratio sulfur / butadiene 1.46mol, water / butadiene 1.8mol, reaction residence time 1.54s. The output is 4600Kg per day. The unit consumption of butadiene is 0.87 tons, and the yield is 74%. However, the temperature of the tar kettle is high, and coking occurs quickly, and it takes only 5 days to shut down for cleaning.

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Abstract

The invention relates to method and device for producing thiophene by synthesizing butadiene and sulfur. The production method comprises the steps of reaction, separation and desulfurization. In the reaction process, raw materials are heated to initial reaction temperature by a water hose heat and intermediate frequency induction heating method, but a reactor does not need to be heated; the reaction is carried out under normal pressure at the temperature of 380-450 DEG C; the molar ratio of the sulfur to the butadiene is 1.2-1.6, the molar ratio of water to the butadiene is 1-2, and the retention time of the reaction is 1-2 seconds. A multistage cooling method is adopted to separate high boiling point tar and unreacted sulfur in a reaction product, thereby solving the problem of blockagesof pipelines and equipment. A freezing and absorbing method is adopted to recover thiophene in hydrogen sulfide which is tail gas, thereby improving the yield of the thiophene. Methods of vapor pressure sealing emptying and two-stage wet desulfurizing are adopted, thereby solving pollution problems of the tar and the hydrogen sulfide in a production process and realizing the cleaning production of the thiophene.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a production method and device for thiophene and its derivatives. Background technique [0002] Thiophene, also known as thiolane and thiofuran, is the most important sulfur heterocyclic compound and an important organic chemical raw material. It is often used as a reagent for organic synthesis and is widely used in the synthesis of dyes, medicines, pesticides, and polymer additives. Wait. Especially as an important pharmaceutical raw material, thiophene can be used to synthesize hundreds of drugs such as cephalosporins and cephalosporins. There are two types of derivatives of thiophene: α-position (2, 5-position) and β-position (3, 4-position). The α-position is larger than the β-position derivative and has more varieties, but the β-position derivative is expensive, even up to 1000 ten thousand yuan / ton. [0003] The earliest production method of thiophene is to extract from the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/10C07D333/08C07D333/28B01D53/48B01D53/52B01D53/78B01D53/14
Inventor 杨顺立
Owner LIANYUNGANG DIPU CHEM
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