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Method for continuously preparing 1, 4-dichlorobutane

A technology for dichlorobutane and preparation steps, which is applied in the field of continuous preparation of 1,4-dichlorobutane, can solve problems such as increasing production cost, and achieve the effects of less waste generation, less side reactions, and improved dispersibility

Pending Publication Date: 2021-11-12
CHINA SALT CHANGZHOU CHEM
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Instead of a large amount of hydrogen chloride by-products in the chlorination process, it is easy to entrain a small amount of organic matter when used as a by-product acid, and the organic matter needs to be treated to less than 50ppm before it can be sold as a product, thus greatly increasing the production cost

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  • Method for continuously preparing 1, 4-dichlorobutane

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preparation example Construction

[0027] The preparation process of the 1,4-dichlorobutane is:

[0028] (1) Add tetrahydrofuran into the enhanced reactor and preheat to 93-97°C;

[0029] (2) Heat the intensified reactor to 120-150°C, then slowly feed the amount of hydrogen chloride into the intensified reactor according to the molar ratio of tetrahydrofuran to hydrogen chloride: 1:2.05-2.1, and control the pressure in the intensified reactor to 1.2-1.5MPa , forced circulation reaction, sampling and analysis every 0.5h during the reaction process, stop the reaction when the conversion rate of tetrahydrofuran reaches 85-95%, and obtain the reaction solution;

[0030] (3) Add the reaction liquid obtained in step (2) into the first rectification tower, control the temperature of the first rectification tower tower bottom to be 25~60°C, and the pressure of the first rectification tower to be -0.09~-0.05Mpa, the rectification process Hydrogen chloride and tetrahydrofuran fractions are recovered at the top of the to...

Embodiment 1

[0034] A method for continuously preparing 1,4-dichlorobutane. The enhanced reactor is a pipe reactor with an inner diameter of φ100mm and a length of 2.0m with an extracorporeal pumping cycle, and the inner filler is an inert θ ring filler; 1,4- The preparation process of dichlorobutane is:

[0035] (1) adding tetrahydrofuran into the enhanced reactor and preheating to 93°C;

[0036] (2) Heat the enhanced reactor to 120°C, then slowly feed the amount of hydrogen chloride into the enhanced reactor according to the molar ratio of tetrahydrofuran to hydrogen chloride of 1:2.05, and control the pressure of the enhanced reactor to 1.2MPa, forced circulation reaction, reaction Sampling and analysis every 0.5h during the process, stop the reaction when the conversion rate of tetrahydrofuran reaches 85%, and obtain the reaction solution;

[0037] (3) Add the reaction solution obtained in step (2) into the first rectifying tower, control the temperature of the first rectifying tower ...

Embodiment 2

[0040] A method for continuously preparing 1,4-dichlorobutane. The enhanced reactor is a pipe reactor with an inner diameter of φ100mm and a length of 2.0m with an extracorporeal pumping cycle, and the inner filler is an inert θ ring filler; 1,4- The preparation process of dichlorobutane is:

[0041] (1) adding tetrahydrofuran into the enhanced reactor and preheating to 95°C;

[0042] (2) Heat the enhanced reactor to 136°C, then slowly feed the amount of hydrogen chloride into the enhanced reactor according to the tetrahydrofuran:hydrogen chloride molar ratio of 1:2.07, and control the enhanced reactor pressure to 1.35MPa, forced circulation reaction, reaction Sampling and analysis every 0.5h during the process, stop the reaction when the conversion rate of tetrahydrofuran reaches 90%, and obtain the reaction solution;

[0043] (3) Add the reaction solution obtained in step (2) to the first rectification tower, control the temperature of the first rectification tower tower bo...

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Abstract

The invention relates to a method for continuously preparing 1, 4-dichlorobutane, and belongs to the technical field of chemical product preparation. The invention discloses a method for continuously preparing 1, 4-dichlorobutane, and the method comprises the following steps: adding a Lewis acid catalyst into tetrahydrofuran and hydrogen chloride in a reinforced pipeline reactor filled with inert filler, carrying out forced circulation reaction to obtain a crude product, and carrying out reduced pressure rectification twice to obtain the 1, 4-dichlorobutane, wherein tetrahydrofuran mainly obtained at the top of the first rectifying tower can be recycled, and a small amount of catalyst raffinate at the bottom of the second rectifying tower is subjected to high-boiling treatment. The process method provided by the invention is high in material utilization rate, high in product purity, easy in reaction process control and capable of realizing continuous production.

Description

technical field [0001] The invention relates to a method for continuously preparing 1,4-dichlorobutane, which belongs to the technical field of chemical product preparation. Background technique [0002] At present, 1,4-dichlorobutane is an important fine chemical product, which can be used as a raw material and solvent for organic synthesis, and for the synthesis of adiponitrile, the drug kebezemide, etc. There are a lot of hydrogen chloride by-products in the replacement chlorination process, and a small amount of organic matter is easily entrained when the by-product acid is used, and the organic matter needs to be treated to less than 50ppm before it can be sold as a product, thus greatly increasing the production cost. If the by-product hydrogen chloride is simply treated as a raw material for the production of 1,4-dichlorobutane and comprehensively utilized, it can not only turn waste into treasure, but also improve the economy of the process and embody the concept of ...

Claims

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Application Information

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IPC IPC(8): C07C17/00C07C17/383C07C19/01
CPCC07C17/00C07C17/383C07C19/01
Inventor 董亮陶文平马凯王顺利张驰郝祥忠张明吴发明孙运林
Owner CHINA SALT CHANGZHOU CHEM
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