CN220194028U - Continuous purification device of tetrachloro isophthalonitrile - Google Patents

Continuous purification device of tetrachloro isophthalonitrile Download PDF

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Publication number
CN220194028U
CN220194028U CN202320738982.9U CN202320738982U CN220194028U CN 220194028 U CN220194028 U CN 220194028U CN 202320738982 U CN202320738982 U CN 202320738982U CN 220194028 U CN220194028 U CN 220194028U
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dissolution kettle
solvent
stirring
input port
communicates
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张海朋
张正虎
齐凯言
陆政松
张建
刘宗健
逯芹
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Shandong Dacheng Biological Chemical Co ltd
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Shandong Dacheng Biological Chemical Co ltd
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Abstract

The utility model discloses a continuous purification device for tetrachloro isophthalonitrile, and belongs to the technical field of tetrachloro isophthalonitrile purification equipment. The method is characterized in that: including dissolution kettle (1), crystallizer (2), centrifugal filter (3), desicator (4) and solvent circulating device, the delivery outlet of dissolution kettle (1) communicates with the input port of crystallizer (2), the delivery outlet of crystallizer (2) communicates with the input port of centrifugal filter (3), the solid phase export of centrifugal filter (3) communicates with the input port of desicator (4), the liquid phase export of centrifugal filter (3) communicates with the input port of solvent circulating device, solvent circulating device's delivery outlet communicates with dissolution kettle (1). The continuous purification device for the tetrachloro isophthalonitrile adopts a recrystallization method to purify the tetrachloro isophthalonitrile, so that the content of hexachlorobenzene in the purified tetrachloro isophthalonitrile is less than 10ppm, and the operation cost is greatly reduced.

Description

Continuous purification device of tetrachloro isophthalonitrile
Technical Field
A continuous purification device of tetrachloro isophthalonitrile belongs to the technical field of tetrachloro isophthalonitrile purification equipment.
Background
Chlorothalonil (tetrachloro isophthalonitrile) is a broad-spectrum, efficient, low-toxicity and low-residue agricultural and forest protective bactericide, is not easy to generate drug resistance, and is widely applied to prevention and treatment of fruits, vegetables and leaves, such as: various fungal diseases of crops such as vegetables, fruits, beans, rice, wheat and the like. In the industrial production of chlorothalonil, a high-temperature gas phase method is mainly adopted, isophthalonitrile and chlorine are used as raw materials, the isophthalonitrile solid raw materials are melted and vaporized at high temperature, meanwhile, chlorine is introduced at high temperature to react at high temperature in the presence of an active carbon catalyst, and the obtained reaction gas is cooled and sublimated to finally obtain the chlorothalonil product. The production scale of chlorothalonil in China is continuously expanding, 6-ten thousand-ton-level excellent pesticides are produced in year at present, and the chlorothalonil is in a marketable state in the international market all the time. The chlorothalonil is defined in national standard GB/T9551-2017 in China as white powder, the main content of the chlorothalonil is more than or equal to 97%, and the hexachlorobenzene content is less than or equal to 40 ppm. However, in the production of chlorothalonil, 5% -15% of products are often caused by the start and stop of the reaction period, and the products are caused by the main content and the hexachlorobenzene content. It is of great significance to develop a new purification process to convert this fraction of reject product into a acceptable product.
Hexachlorobenzene (HCB) contained in chlorothalonil is a substance harmful to human bodies, is difficult to degrade in natural environments, and is easy to accumulate in organisms and in environments. In order to protect the environment and ensure the health of human bodies, FAO standard of international grain and agricultural organization is listed as an important control project, so that the hundred-bacteria purification process is required to be researched and developed, on one hand, partial unqualified products are purified into qualified products, the production unit consumption is reduced, and on the other hand, the HCB content in the products is reduced to below 5ppm to meet the market demand.
In the prior art, most of the chlorothalonil is purified by adopting a rectification method, the produced chlorothalonil product is put into a heating kettle, the produced chlorothalonil product is heated and melted by adopting heat conduction oil, the temperature of the heat conduction oil is up to 260-350 ℃, the melted chlorothalonil enters a superheating device to be vaporized for rectification, light components are extracted from the top of a rectifying tower and enter a front cut trapping device to be sublimated; the heavy components are extracted from the bottom of the rectifying tower and enter a refining kettle, and solid chlorothalonil is obtained after condensation. The method can only treat materials with the main content of 90% -95%, the chlorothalonil with lower content is difficult to treat, the surface of the heater is vaporized due to long-time high-temperature vaporization, and periodic deslagging is needed.
CN108329235a discloses a process method for producing high-purity chlorothalonil, which adopts a rectification process method as well. The method comprises the steps of feeding raw materials of chlorothalonil, isophthalonitrile, trichloroisophthalonitrile, pentachlorobenzonitrile, hexachlorobenzene and water into a light component removing tower. A step of extracting a mixture of chlorothalonil with the weight content of light components being less than or equal to 0.01% and heavy components from the bottom of the light component removal tower, then sending the mixture into a product tower, and extracting a chlorothalonil product with the weight content being more than or equal to 99.5% from the top of the product tower; the mass fraction of chlorothalonil in the raw materials is 87-96%; the light component comprises isophthalonitrile, trichloroisophthalonitrile and hexachlorobenzene; the heavy component comprises pentachlorobenzonitrile and tar with the mass content not higher than 0.05 percent. According to the process method for producing high-purity chlorothalonil, disclosed by the utility model, the chlorothalonil is refined by adopting a rectification process, the operation process is simple, and a chlorothalonil product with the mass fraction of more than 99.5% can be obtained. However, the method adopts double-tower continuous rectification to refine and purify the chlorothalonil, increases the investment cost of the system, is not beneficial to industrialized popularization, and aims at the problem that the chlorothalonil content range in the chlorothalonil treatment raw material is narrow, and the operation elasticity and the operable space are not large. And meanwhile, a great amount of fuel is wasted by a heating rectification method.
Disclosure of Invention
The utility model aims to solve the technical problems that: overcomes the defects of the prior art, and provides a continuous purifying device for the tetrachloro isophthalonitrile, which can continuously purify the tetrachloro isophthalonitrile, can adapt to the purification of tetrachloro isophthalonitrile with different concentrations and has low operation cost.
The technical scheme adopted for solving the technical problems is as follows: this continuous purification device of tetrachloro isophthalonitrile, its characterized in that: the device comprises a dissolution kettle, a crystallizer, a centrifugal filter, a dryer and a solvent circulating device, wherein an output port of the dissolution kettle is communicated with an input port of the crystallizer, an output port of the crystallizer is communicated with an input port of the centrifugal filter, a solid phase outlet of the centrifugal filter is communicated with an input port of the dryer, a liquid phase outlet of the centrifugal filter is communicated with an input port of the solvent circulating device, and an output port of the solvent circulating device is communicated with the dissolution kettle.
Preferably, the solvent circulating device comprises a falling film evaporator and a condenser, wherein an input port of the falling film evaporator is communicated with a liquid phase outlet of the centrifugal filter, a gas phase outlet of the falling film evaporator is communicated with an input port of the condenser, and an output port of the condenser is communicated with the dissolution kettle.
Preferably, the device further comprises a solvent tank, an output port of the solvent circulating device is communicated with the solvent tank, an output port of the solvent tank is communicated with the dissolution kettle, and the solvent tank is further connected with a solvent adding pipe.
Preferably, the device further comprises a metering tank, wherein an input port of the metering tank is communicated with an output port of the solvent tank, and an output port of the metering tank is communicated with the dissolution kettle.
Preferably, the dissolution kettle comprises a dissolution kettle body, a jacket arranged around the dissolution kettle body and a stirring device, wherein the stirring device is arranged in the dissolution kettle body.
Preferably, the stirring device comprises a stirring motor, a stirring shaft and stirring paddles, wherein the stirring shaft is vertically arranged in the dissolution kettle main body, an output shaft of the stirring motor is connected with the stirring shaft, and the stirring paddles are provided with a plurality of stirring paddles around the stirring shaft.
Preferably, the stirring blade is inclined upwards gradually along the direction approaching the stirring shaft.
Preferably, a baffle is arranged in the jacket, the baffle is spiral and is arranged around the main body of the dissolution kettle, and a spiral heating channel is formed in the jacket.
Compared with the prior art, the utility model has the following beneficial effects:
the dissolving kettle of the continuous purifying device for the tetrachloro isophthalonitrile dissolves the tetrachloro isophthalonitrile, and then carries out a cooling crystallization mode, namely, the purifying of the tetrachloro isophthalonitrile is realized in a recrystallization mode, the concentration requirement on the tetrachloro isophthalonitrile before purification is low, the hexachlorobenzene content in the purified tetrachloro isophthalonitrile is less than 10ppm, and compared with the purifying mode of the tetrachloro isophthalonitrile by adopting a rectification mode, the operating cost is greatly reduced.
Drawings
FIG. 1 is a schematic diagram showing the structure of a continuous purification apparatus for tetrachloro isophthalonitrile.
FIG. 2 is a schematic diagram of a cross-sectional front view of a dissolution vessel.
In the figure: 1. the dissolution kettle 2, the crystallizer 3, the centrifugal filter 4, the dryer 5, the falling film evaporator 6, the stirring motor 7, the condenser 8, the solvent tank 9, the metering tank 10, the kettle body 11, the jacket 12, the baffle 13, the discharging pipe 14, the stirring shaft 15 and the stirring blade.
Detailed Description
The present utility model will be further described with reference to specific embodiments, however, it will be appreciated by those skilled in the art that the detailed description herein with reference to the accompanying drawings is for better illustration, and that the utility model is not necessarily limited to such embodiments, but rather is intended to cover various equivalent alternatives or modifications, as may be readily apparent to those skilled in the art.
Fig. 1-2 are diagrams illustrating a preferred embodiment of the present utility model, and the present utility model is further described with reference to fig. 1-2.
The utility model provides a continuous purification device of tetrachloro isophthalonitrile, including dissolution kettle 1, crystallizer 2, centrifugal filter 3, desicator 4 and solvent circulating device, the delivery outlet of dissolution kettle 1 communicates with the input port of crystallizer 2, the delivery outlet of crystallizer 2 communicates with the input port of centrifugal filter 3, the solid phase export of centrifugal filter 3 communicates with the input port of desicator 4, the liquid phase export of centrifugal filter 3 communicates with solvent circulating device's input port, solvent circulating device's delivery outlet communicates with dissolution kettle 1. The dissolving kettle 1 of the continuous purifying device for the tetrachloro isophthalonitrile dissolves the tetrachloro isophthalonitrile, then carries out a cooling crystallization mode, realizes the purification of the tetrachloro isophthalonitrile, has low requirement on the concentration of the tetrachloro isophthalonitrile before purification, can ensure that the content of hexachlorobenzene in the purified tetrachloro isophthalonitrile is less than 10ppm, and greatly reduces the operation cost compared with the mode of purifying the tetrachloro isophthalonitrile by adopting a rectification mode.
Specific: as shown in fig. 1: the top of dissolution kettle 1 is provided with charge door and liquid filling opening, and the delivery outlet of dissolution kettle 1 sets up in the bottom of dissolution kettle 1, and the delivery outlet of dissolution kettle 1 communicates with the input port of crystallizer 2, and the crystallizer 2 adopts tower crystallizer, and crystallizer 2 adopts the mode of carrying out cooling crystallization to the solution, makes tetrachloro isophthalonitrile crystallization separate out. The solid phase outlet of the crystallizer 2 is communicated with the input port of the dryer 4, and the dryer 4 dries the solid material to obtain a high-quality chlorothalonil product with the hexachlorobenzene content of less than 10 ppm.
The input port of the liquid phase outlet solvent circulating device of the centrifugal filter 3 is communicated, the output port of the solvent circulating device is communicated with the liquid adding port of the dissolution kettle 1, so that the solvent can be recycled, and the loss of the solvent in the running process of the equipment is reduced.
The solvent circulating device comprises a falling film evaporator 5 and a condenser 7, wherein the input port of the falling film evaporator 5 is communicated with the liquid phase outlet of the centrifugal filter 3, the gas phase outlet of the falling film evaporator 5 is communicated with the input port of the condenser 7, solvent steam is sent into the condenser 7 to be condensed and liquefied, and the solvent condensed in the condenser 7 is sent into the dissolution kettle 1.
The continuous purification device of the tetrachloro isophthalonitrile further comprises a solvent tank 8 and a metering tank 9, wherein an input port of the solvent tank 8 is communicated with an output port of the condenser 7, the condensed and liquefied solvent of the condenser 7 enters the solvent tank 8, an output port of the solvent tank 8 is communicated with an input port of the metering tank 9, and an output port of the metering tank 9 is communicated with a liquid adding port of the dissolution kettle 1.
The condensed and liquefied solvent in the condenser 7 enters the solvent tank 8 for storage, and the solvent in the solvent tank 8 is fed into the dissolution kettle 1 after being measured by the measuring tank 9, so that the amount of the solvent added into the dissolution kettle 1 is conveniently and accurately controlled. The solvent tank 8 is used for storing the solvent, and a solvent adding pipe is connected to the solvent tank 8 to add the solvent into the solvent tank 8.
As shown in fig. 2: the dissolution kettle 1 comprises a dissolution kettle body, a stirring device and a jacket 11, wherein the dissolution kettle body comprises a kettle body 10, and a discharging pipe 13 is arranged at the bottom of the kettle body 10 so as to facilitate the delivery of dissolved materials. The stirring device is arranged in the kettle body 10, the jacket 11 is arranged around the kettle body 10, the kettle body 10 can be heated through the jacket 11, so that the temperature of the kettle body 10 is increased, the dissolution speed can be increased, the subsequent cooling crystallization is convenient, and the stirring device can stir the solvent and the tetrachloro isophthalonitrile, so that the dissolution speed is further increased.
The baffle 12 is arranged in the jacket 11, the baffle 12 is in a spiral shape coaxial with the kettle body 10, so that a spiral heating channel is formed in the jacket 11, steam for heating the kettle body 10 can flow through the inner wall of the kettle body 10, so that the kettle body 10 is comprehensively heated, and the kettle body 10 is heated more uniformly.
Stirring device includes agitator motor 6, (mixing) shaft 14 and stirring paddle 15, agitator motor 6 installs at the top of the cauldron body 10, the vertical setting of (mixing) shaft 14 is in the cauldron body 10, rotatable and the cauldron body 10 of upper end of (mixing) shaft 14 are connected, agitator motor 6's output shaft and (mixing) shaft 14 are connected, agitator motor 6 drives (mixing) shaft 14 and rotates, stirring paddle 15 encircles (mixing) shaft 14 interval and is provided with a plurality of, and then has realized the stirring to the material in the cauldron body 10 through (mixing) shaft 14 and stirring paddle 15) to make the quick solution of tetrachloroisophthalonitrile.
Further, the stirring blades 15 are inclined gradually upward in the direction approaching the stirring shaft 14, so that the stirring range of the stirring blades 15 can be increased, and each stirring blade 15 can stir not only in the radial direction of the tank 10 but also in the depth direction of the tank 10.
According to the continuous purification device for the tetrachloro isophthalonitrile, unqualified chlorothalonil products with the main content of 75% -97% are removed by adopting a recrystallization method, and impurities such as hexachlorobenzene, unreacted isophthalonitrile, hydrochloric acid, rust and the like are removed, so that high-quality chlorothalonil products with the main content of more than or equal to 99% and the hexachlorobenzene content of less than 10ppm are obtained.
And heating and dissolving the unqualified chlorothalonil product by water or a mixed solution of water and an organic solvent, regulating the pH value to be less than or equal to 1 by using a small amount of acid, cooling, carrying out solid-liquid separation, and drying to obtain a solid chlorothalonil product.
The low-content chlorothalonil product is heated and dissolved by water or mixed liquid of water and an organic solvent, and the quality of the product is improved by a recrystallization mode; the organic solvent is one or a combination of at least two of dichloromethane, chloroform, toluene, m-xylene or acetone, preferably dichloromethane and toluene, and the toluene and water are further optimally selected for sharing. The pH value is adjusted to be less than or equal to 1 by adopting concentrated acid, and concentrated sulfuric acid is further preferred.
The above description is only a preferred embodiment of the present utility model, and is not intended to limit the utility model in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present utility model still fall within the protection scope of the technical solution of the present utility model.

Claims (8)

1. A continuous purification device of tetrachloro isophthalonitrile is characterized in that: including dissolution kettle (1), crystallizer (2), centrifugal filter (3), desicator (4) and solvent circulating device, the delivery outlet of dissolution kettle (1) communicates with the input port of crystallizer (2), the delivery outlet of crystallizer (2) communicates with the input port of centrifugal filter (3), the solid phase export of centrifugal filter (3) communicates with the input port of desicator (4), the liquid phase export of centrifugal filter (3) communicates with the input port of solvent circulating device, solvent circulating device's delivery outlet communicates with dissolution kettle (1).
2. The continuous purification device of tetrachloroisophthalonitrile according to claim 1, wherein: the solvent circulating device comprises a falling film evaporator (5) and a condenser (7), wherein an input port of the falling film evaporator (5) is communicated with a liquid phase outlet of the centrifugal filter (3), a gas phase outlet of the falling film evaporator (5) is communicated with an input port of the condenser (7), and an output port of the condenser (7) is communicated with the dissolution kettle (1).
3. The continuous purification device of tetrachloroisophthalonitrile according to claim 1, wherein: still include solvent tank (8), solvent circulation device's delivery outlet and solvent tank (8) intercommunication, solvent tank (8)'s delivery outlet and dissolution kettle (1) intercommunication, solvent tank (8) still are connected with solvent and add the pipe.
4. The continuous purification apparatus for tetrachloroisophthalonitrile according to claim 1 or 3, wherein: the device also comprises a metering tank (9), wherein an input port of the metering tank (9) is communicated with an output port of the solvent tank (8), and an output port of the metering tank (9) is communicated with the dissolution kettle (1).
5. The continuous purification device for tetrachloroisophthalonitrile according to any one of claims 1 to 3, wherein: the dissolution kettle (1) comprises a dissolution kettle main body, a jacket (11) arranged around the dissolution kettle main body and a stirring device, wherein the stirring device is arranged in the dissolution kettle main body.
6. The continuous purification apparatus for tetrachloroisophthalonitrile according to claim 5, wherein: the stirring device comprises a stirring motor (6), a stirring shaft (14) and stirring blades (15), wherein the stirring shaft (14) is vertically arranged in the dissolution kettle main body, an output shaft of the stirring motor (6) is connected with the stirring shaft (14), and the stirring blades (15) are arranged around the stirring shaft (14) in a plurality.
7. The continuous purification apparatus for tetrachloroisophthalonitrile according to claim 6, wherein: the stirring blade (15) is inclined upwards gradually along the direction approaching the stirring shaft (14).
8. The continuous purification apparatus for tetrachloroisophthalonitrile according to claim 5, wherein: the jacket (11) is internally provided with a baffle plate (12), the baffle plate (12) is in a spiral shape arranged around the main body of the dissolution kettle, and a spiral heating channel is formed in the jacket (11).
CN202320738982.9U 2023-04-06 2023-04-06 Continuous purification device of tetrachloro isophthalonitrile Active CN220194028U (en)

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CN202320738982.9U CN220194028U (en) 2023-04-06 2023-04-06 Continuous purification device of tetrachloro isophthalonitrile

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Application Number Priority Date Filing Date Title
CN202320738982.9U CN220194028U (en) 2023-04-06 2023-04-06 Continuous purification device of tetrachloro isophthalonitrile

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CN220194028U true CN220194028U (en) 2023-12-19

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