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A trapping device and process for the production of 3,4-dichlorobenzonitrile

A dichlorobenzonitrile and process technology, which is applied in the field of trapping devices for the production of 3,4-dichlorobenzonitrile, can solve the problems of difficult cooling of circulating spray water, harsh working environment, and large amount of waste water, and achieve Reduce the workload of distillation and purification, the structure design is simple and reasonable, and realize the effect of recycling

Active Publication Date: 2021-03-26
常州新日催化剂股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patents CN201384868Y and CN101954231B both adopt the water spray capture method. The biggest problem of this capture method is that the amount of wastewater to be treated is large, the cost of wastewater treatment is high, and it is difficult to cool down the circulating spray water
Chinese patent CN101955447B adopts the method of solvent capture, which needs to add additional organic solvents, and the energy consumption of two-stage rectification is high
At present, the domestic production of aromatics with nitrile groups and halogenated aromatics by the ammonia oxidation method is mainly thin-walled capture. This capture method is labor-intensive for workers and the working environment on site is harsh, and continuous discharge of products cannot be achieved. , a large amount of wastewater treatment

Method used

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  • A trapping device and process for the production of 3,4-dichlorobenzonitrile
  • A trapping device and process for the production of 3,4-dichlorobenzonitrile
  • A trapping device and process for the production of 3,4-dichlorobenzonitrile

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Experimental program
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Effect test

Embodiment 1

[0036] Such as figure 1 Shown, the present invention is a kind of trapping device that is used for 3,4-dichlorobenzonitrile production, comprises primary trap, secondary trap, tertiary trap, washing tower, rectifying tower , product tank, waste water treatment device and tail gas treatment device, the 3,4-dichlorobenzonitrile high-temperature mixed product from the reactor enters the primary trap through the feed inlet of the primary trap, and a The gas outlet at the top of the primary trap is connected to the feed port of the secondary trap, and the gas outlet at the top of the secondary trap is connected to the feed port of the tertiary trap. The gas outlet at the top of the stage trap is connected to the inlet of the water washing tower, and the gas outlet at the top of the water washing tower is connected to the tail gas treatment device;

[0037] The discharge port at the bottom of the primary trap is connected to the feed port of the first melting layered tank, the disc...

Embodiment 2

[0053] The difference between embodiment 2 and embodiment 1 is that (two) trapping section:

[0054] S1: The high-temperature mixed product of 3,4-dichlorobenzonitrile from the reactor enters the primary trap. At this time, the cold medium spray device sprays The cooling medium is evaporated and cooled, 54.69g of ammonium chloride solid and 34.2g of 3,4-dichlorobenzonitrile liquefaction condensation are precipitated in the primary trap, and the solid-liquid mixture produced in the primary trap is heated at 500g at 50°C Water dissolves, washes and stratifies, in which the upper aqueous phase is cooled and crystallized and centrifuged to separate the ammonium chloride solid product and centrifugate, the centrifugate is used as a solvent for the solid-liquid mixture generated in the primary trap, and the lower organic phase is sent to the separation Layer device, after washing with water for many times, the liquid product of 3,4-dichlorobenzonitrile with a purity ≥ 99.5% is obtai...

Embodiment 3

[0060] The difference between embodiment 3 and embodiment 1 is that (two) trapping section:

[0061] S1: The high-temperature mixed product of 3,4-dichlorobenzonitrile from the reactor enters the primary trap. At this time, the cold medium spray device sprays The cooling medium is evaporated and cooled, and 77.62g of ammonium chloride solid and 91.2g of 3,4-dichlorobenzonitrile liquefaction condensation are precipitated in the primary trap. Water dissolves, washes and stratifies, in which the upper aqueous phase is cooled and crystallized and centrifuged to separate the ammonium chloride solid product and centrifugate, the centrifugate is used as a solvent for the solid-liquid mixture generated in the primary trap, and the lower organic phase is sent to the separation Layer device, after washing with water for many times, the liquid product of 3,4-dichlorobenzonitrile with a purity ≥ 99.5% is obtained, and the mixed product atmosphere after the initial cooling of the primary t...

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Abstract

The invention discloses a trapping device and process for production of 3,4-dichlorobenzonitrile. The device is simple and reasonable in structural design; the implementation feasibility is high, thepracticability is high, more than 90% of ammonium chloride and more than 8% of 3,4-dichlorobenzonitrile are captured by a first-stage catcher through a dry capture method, more than 76% of 3,4-dichlorobenzonitrile is captured by a second-stage catcher through a dry capture method, latent heat of vaporization of water is fully utilized by the first-stage catcher, and the usage amount of spray liquid-water is small; besides, about 15% of the 3,4-dichlorobenzonitrile crude product collected by a third-stage catcher and a bath tower is dissolved by hot water, dehydrated, rectified and purified toobtain a liquid pure product of 3,4-dichlorobenzonitrile. The generation amount of coke oil and solid waste during the rectification process is low. Compared with a traditional multi-stage wet capturemethod, the consumption of 3,4-dichlorobenzonitrile is reduced, the investment cost of rectification equipment is reduced by more than half, the rectification energy consumption is equivalent to 15%of that of the traditional method, and the economic benefit is good.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a trapping device and process for the production of 3,4-dichlorobenzonitrile. Background technique [0002] 3,4-Dichlorobenzonitrile (abbreviated as 3,4-DCN) is an important organic raw material for the synthesis of the selective herbicide cyhalofop; its 3,4-difluorobenzonitrile synthesized by fluorination is an important Organic fluorine pesticide intermediates; in addition, it can also be widely used as intermediates in medicine, pigments, dyes, and liquid crystal materials. [0003] As the patent protection of cyhalofop developed by Dow AgroSciences of the United States expires, research on its production method has been launched in various countries, which has led to an increasing demand for the raw material 3,4-dichlorobenzonitrile. [0004] In 3,4-dichlorobenzonitrile synthesis technology, disclosed in EP441004 by 3,4-dichloromethylbenzene and NH 4 Cl reaction ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/34C07C253/32C07C255/50B01D3/14
CPCB01D3/143C07C253/28C07C255/50
Inventor 刘先国胡佳魏士新王康军邹红旭陈鹏徐伟金亮
Owner 常州新日催化剂股份有限公司
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