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A kind of method and device of crude pyridine refining high-purity pyridine series products

A series of products, pyridine technology, applied in the field of coal chemical industry, can solve the problems that the production process cannot be carried out smoothly, trace moisture cannot be removed, plugging packing and reboiler, etc., so as to reduce equipment investment and process energy consumption, reduce investment and Effects of energy consumption, simplification of processes and equipment

Active Publication Date: 2022-07-29
CHINA CONSTR IND & ENERGY ENG GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Current research mainly focuses on the simple separation of phenolic compounds or the simultaneous separation of phenolic compounds and pyridine compounds. For example, the domestic patent CN102731264 discloses a continuous distillation to obtain two high-purity phenolic products and one high-content mixed phenolic product. A method for separating crude phenols from medium and low temperature coal tar, and CN107721826 further discloses a method and device for separating various phenols from crude phenols from medium and low temperature coal tar. The crude phenol products are mainly obtained through a pretreatment system, and the crude phenol products are then processed through continuous Four kinds of high-purity phenol series products are obtained by the rectification system; and the domestic patent CN104893750 discloses a method for extracting pyridine compounds from coal tar. Phenolic compounds and dephenolized oil, and then use solvent extraction to extract all the crude pyridine compounds in the phenolic compounds and dephenolized oil, and finally obtain pyridine compounds through dehydration, slag removal and rectification; although there are many studies, but There is no specific method on how to refine high-purity pyridine series products from pyridine compounds. Therefore, it is of great significance to separate and refine high-purity pyridine series products from medium and low temperature coal tar crude pyridine
[0004] The existing process of producing pyridine from coal tar has the disadvantage of not being able to remove trace moisture, but the existence of trace moisture will greatly affect product quality
In addition, coal tar crude pyridine raw materials generally contain residues with a mass percentage of about 3%. In addition to high boiling point components (boiling point more than 225 ° C), it also contains Na2SO4, Na2CO3 and other inorganic salts. If it is not removed first, it will be directly used If the continuous tower is used, the packing and reboiler will inevitably be blocked, and the production process cannot be carried out smoothly.

Method used

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  • A kind of method and device of crude pyridine refining high-purity pyridine series products

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Embodiment 1

[0031] Embodiment 1: a kind of method of crude pyridine refining high-purity pyridine series product, may further comprise the steps:

[0032] S1, mix the crude pyridine raw material from medium and low temperature coal tar with part of the azeotroping agent, utilize low-pressure steam or other low-temperature heat sources to enter drying tower T101 after preheating through drying tower T101 feed preheater 1; The raw material flow rate of pyridine is 8421kg / h, the pressure is 0.4MPa and the temperature is 40℃, and its mass composition is water 6.5%, benzene 15.0%, pyridine 40.5%, o-methylpyridine 3.7%, 2,6-lutidine 3.5% %, m-picoline 7%, o-ethylpyridine 0.3%, 2,4-lutidine 7%, 2,3,6-collidine 6%, indane 0.1%, aniline 5.8%, benzyl Amine 2.4%, m-toluidine 2% and quinoline 0.2%.

[0033] S2, adopt azeotropic rectification technology, carry out azeotropic rectification through drying tower T101, the gas phase at the top of drying tower T101 is condensed by drying tower T101 conden...

Embodiment 2

[0043] Embodiment 2: In this embodiment, the crude pyridine raw material flow rate is 8421kg / h, the pressure is 0.4MPa and the temperature is 40°C, and its mass composition is water 8%, benzene 10.0%, pyridine 46%, o-methylpyridine 3%. %, 2,6-lutidine 3.2%, m-methylpyridine 5%, o-ethylpyridine 0.3%, 2,4-lutidine 8%, 2,3,6-collidine 6% , indane 0.1%, aniline 5.8%, benzylamine 2.4%, m-toluidine 2% and quinoline 0.2%; other technological processes are the same as in Example 1, and the pyridine tower T104 tower top obtains 3874kg / h and the purity is 99.5wt% pyridine product, the pyridine tower T104 tower still obtains 232kg / h of o-methylpyridine product whose purity is 99.8wt%; the methylpyridine tower T105 obtains 711kg / h content exceeding 96.5wt% picoline product mixture material, dimethyl pyridine The pyridine tower T106 was refined to obtain 671kg / h of 2,4-lutidine with a purity of 99.8wt%, and 498kg / h of 2,3,6-trimethylpyridine with a purity of 98.3wt% was extracted from the ...

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Abstract

The invention discloses a method for purifying high-purity pyridine series products from crude pyridine. The water phase and the entrainer are obtained, the entrainer is recycled or extracted for later use, and the crude pyridine material is obtained by drying the tower reactor; (2) Deweighting: the crude pyridine material obtained in step (1) enters the evaporating kettle for deweighting treatment , the vapor phase part of the top of the evaporation kettle returns to the drying tower, and the other part enters the pre-fractionation tower for light and heavy material fractionation; (3) rectification of pyridine series products. The invention adopts azeotropic distillation, atmospheric and vacuum distillation and heat integration technology to separate high value-added pyridine series products, so that the purity of pyridine, o-methylpyridine, methylpyridine, lutidine and collidine can reach more than 96wt%, forming an energy-saving and efficient technical method for refining high-purity pyridine series products from crude pyridine.

Description

technical field [0001] The invention belongs to the technical field of coal chemical industry, and particularly relates to a method and a device for refining high-purity pyridine series products from crude pyridine. Background technique [0002] Coal tar is a very valuable chemical raw material, and medium and low temperature coal tar contains a certain amount of crude pyridine and crude phenolic raw materials, such as pyridine, o-methylpyridine, lutidine, collidine and other crude pyridine compounds and Phenol, o-cresol, m-cresol, p-cresol, xylenol, ethyl phenol, tricresol and other crude phenolic compounds, although the content of these compounds is not very high, but they are all high value-added fine chemical products, and synthetic Such substances require high environmental or economic costs. [0003] At present, the research mainly focuses on the simple separation of phenolic compounds or the simultaneous separation of phenolic compounds and pyridine compounds. For ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/16
CPCY02P20/10
Inventor 王佳兵杨万典刘勇军岳昌海陶荣秦凤祥倪明周俊超
Owner CHINA CONSTR IND & ENERGY ENG GRP CO LTD