CN109293529B - Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm - Google Patents
Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm Download PDFInfo
- Publication number
- CN109293529B CN109293529B CN201811486502.4A CN201811486502A CN109293529B CN 109293529 B CN109293529 B CN 109293529B CN 201811486502 A CN201811486502 A CN 201811486502A CN 109293529 B CN109293529 B CN 109293529B
- Authority
- CN
- China
- Prior art keywords
- product
- chlorothalonil
- temperature
- purification apparatus
- melting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000005747 Chlorothalonil Substances 0.000 title claims abstract description 126
- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 title claims abstract description 126
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 73
- 239000002994 raw material Substances 0.000 claims abstract description 57
- 238000000746 purification Methods 0.000 claims abstract description 55
- 238000002844 melting Methods 0.000 claims description 74
- 230000008018 melting Effects 0.000 claims description 74
- 238000000034 method Methods 0.000 claims description 43
- 239000000463 material Substances 0.000 claims description 37
- 239000010963 304 stainless steel Substances 0.000 claims description 36
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 36
- 229910000934 Monel 400 Inorganic materials 0.000 claims description 20
- OANFWJQPUHQWDL-UHFFFAOYSA-N copper iron manganese nickel Chemical compound [Mn].[Fe].[Ni].[Cu] OANFWJQPUHQWDL-UHFFFAOYSA-N 0.000 claims description 20
- 229910000856 hastalloy Inorganic materials 0.000 claims description 20
- 239000000155 melt Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 8
- 239000010962 carbon steel Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims 1
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 123
- 239000007789 gas Substances 0.000 description 18
- 239000007787 solid Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 208000031888 Mycoses Diseases 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a purifying device and a purifying method for producing chlorothalonil with the hexachlorobenzene content not exceeding 10ppm, wherein the purifying device comprises a raw material supply unit, a purifying unit and a product collecting unit which are connected in sequence; the purification unit comprises a rectifying tower, a refining kettle and a condenser, wherein a bottom discharge hole of the rectifying tower is connected with a feed inlet of the refining kettle, and a discharge hole of the refining kettle is connected with a feed inlet of the condenser. According to the invention, the rectifying tower is combined with the refining kettle, and the chlorothalonil with the hexachlorobenzene content of 10-100ppm is refined by using the rectifying kettle after being rectified by the rectifying tower, so that the hexachlorobenzene content in the chlorothalonil product is reduced to be less than 10ppm, the chlorothalonil content in the chlorothalonil product can reach 99.7%, and the purifying device provided by the invention can be used for continuous production and has low operation cost.
Description
Technical Field
The invention belongs to the field of pesticide production, relates to a purification device, in particular to a device and a method for producing chlorothalonil, and particularly relates to a device and a method for producing chlorothalonil with hexachlorobenzene of not more than 10 ppm.
Background
The chlorothalonil is a protective bactericide with high efficiency, low toxicity, broad spectrum and low residue, is widely applied to the prevention and treatment of fungal diseases in agriculture and forestry, and is particularly applied to economic crops such as vegetables, fruits and the like. It is reported by Japanese data that chlorothalonil has a preventive effect on fifty-two diseases of thirty-more crops. In addition, chlorothalonil has important application in the mildew-proof industry field, such as mildew-proof paint, mildew-proof wallpaper, mildew-proof of electric appliances, pi Ping, timber and the like. The production scale of chlorothalonil is continuously enlarged in China, and the chlorothalonil becomes one of large-tonnage good pesticide varieties in the world. Sales in the international market are always in a hot state. The appearance of the chlorothalonil is defined as white powder in national standard GB/T9551-2017 in China, the two main indexes are that the chlorothalonil content is more than or equal to 97wt.% and the hexachlorobenzene content is less than or equal to 40ppm, and the chlorothalonil is qualified. The international market has obviously improved requirements on the inherent quality of chlorothalonil, and besides the content and the appearance, the requirements on the control of harmful substances HCB (hexachlorobenzene) are particularly emphasized, the hexachlorobenzene is not easy to degrade, and the environmental hazard is serious. The international market requires that the content of the chlorothalonil is not more than 10ppm, and the chlorothalonil product with the content of the hexachlorobenzene is developed, wherein the first chlorothalonil occupies the international market, and the second chlorothalonil is reduced in harm to the environment, so that the production of the chlorothalonil with the content of the hexachlorobenzene is not more than 10ppm has important significance.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a purifying device and a purifying method for producing chlorothalonil with the content of hexachlorobenzene not more than 10 ppm.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a purification device for producing chlorothalonil with hexachlorobenzene not exceeding 10ppm, which comprises a raw material supply unit, a purification unit and a product collection unit which are connected in sequence.
The purification unit comprises a rectifying tower, a refining kettle and a condenser, wherein a bottom discharge hole of the rectifying tower is connected with a feed inlet of the refining kettle, and a discharge hole of the refining kettle is connected with a feed inlet of the condenser.
According to the invention, the bottom product of the rectifying tower is refined by arranging the refining kettle, the bottom product of the rectifying tower is a mixture of chlorothalonil, hexachlorobenzene and other heavy components, and the mixture is refined, so that the chlorothalonil product with the hexachlorobenzene content not more than 10ppm can be obtained. The purification device adopted by the invention is simple, the equipment investment is low, and the content of hexachlorobenzene in the obtained chlorothalonil is low.
Preferably, the material of the rectifying tower comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the outer wall of the rectifying tower is provided with a heat tracing pipe. The arrangement of the heat tracing pipe ensures the stability of the temperature in the rectifying tower.
Preferably, a shell and tube condenser is arranged at the top of the rectifying tower.
Preferably, a tubular reboiler is arranged at the bottom of the rectifying tower.
Preferably, the material of the refining kettle comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the outer wall of the refining kettle is provided with a jacket. And heat conduction oil with the temperature of 260-350 ℃ is introduced into the jacket of the refining kettle, and the heat conduction oil heats the materials in the kettle.
Preferably, a coil is arranged in the refining kettle. And heat conduction oil with the temperature of 260-350 ℃ is introduced into the coil pipe of the refining kettle, and the heat conduction oil heats materials in the kettle.
Preferably, the refining kettle is provided with mechanical stirring. The mechanical stirring arrangement can lead the materials in the refining kettle to be heated uniformly.
Preferably, the material of the condenser comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the condenser is a tube array heat exchanger. The shell and tube heat exchanger conducts heat by adopting heat conducting oil with the temperature of 240-330 ℃.
Preferably, the raw material supply unit comprises a raw material bin, a melting kettle, a pipeline filter, a metering pump, a melting middle tank and a superheater which are sequentially connected, wherein a discharge port of the superheater is connected with a feed port of the rectifying tower.
Preferably, the material of the raw material bin comprises carbon steel and/or 304 stainless steel.
Preferably, the material of the melting kettle comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the outer wall of the melting kettle is provided with a jacket. And heat conduction oil with the temperature of 260-350 ℃ is introduced into a jacket of the melting kettle, and the heat conduction oil heats and melts materials in the kettle.
Preferably, the material of the pipe filter includes any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the material of the molten middle tank comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the outer wall of the melting intermediate tank is provided with a jacket. And heat conduction oil with the temperature of 260-350 ℃ is introduced into the jacket of the melting middle tank, and the heat conduction oil heats and melts the materials in the tank.
Preferably, the material of the superheater comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the superheater is a tube array heat exchanger. The superheater heats the material fed from the melt intermediate tank to the bubble point of the material.
Preferably, the material of the metering pump comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the metering pump comprises a plunger metering pump and/or a diaphragm metering pump.
Preferably, the product collecting unit comprises a product receiving kettle, a product catcher and a product vacuum pump, wherein a feed inlet of the product receiving kettle is connected with a discharge outlet of the condenser, a top steam outlet of the product receiving kettle is connected with a feed inlet of the product catcher, and a gas outlet of the product catcher is connected with the product vacuum pump.
Preferably, the material of the product receiving kettle comprises any one of 304 stainless steel, monel 400 or hastelloy.
Preferably, the outer wall of the product receiving kettle is provided with a jacket. And heat conducting oil with the temperature of 240-330 ℃ is introduced into a jacket of the product receiving kettle, and the heat conducting oil heats materials in the kettle.
Preferably, the material of the product catcher comprises carbon steel and/or 304 stainless steel.
Preferably, the outer wall of the product catcher is provided with a jacket. The jacket of the product catcher is filled with water or cold air with the temperature of 40-150 ℃.
Preferably, a baffle is arranged in the product catcher, and the baffle divides the product catcher into two chambers. After the gas with the solid particles is guided by the baffle plate, the solid particles are deposited at the bottom of the product catcher, wherein the deposited solid particles can be used as qualified products.
Preferably, the product vacuum pump comprises any one of a water ring vacuum pump, a piston vacuum pump or a Roots vacuum pump.
Preferably, the purification unit is further provided with a front-end catcher for catching light components produced at the top of the rectifying tower and a front-end vacuum pump connected with a gas outlet of the front-end catcher.
The solid powder trapped in the front cut trap accounts for about 1wt% of the feed amount of the chlorothalonil raw material, is solid waste, and is collected and subjected to centralized treatment.
Preferably, the material of the front cut catcher comprises carbon steel and/or 304 stainless steel.
Preferably, the outer wall of the front cut trap is provided with a jacket. The jacket of the front cut catcher is filled with water or cold air with the temperature of 40-150 ℃.
Preferably, a baffle is arranged in the front fraction catcher, and the baffle divides the front fraction catcher into two chambers. After the solid particles entrained in the gas generated by the melting furnace are guided by the baffle plate, the solid particles are deposited at the bottom of the front fraction catcher, and the solid particles are solid wastes and are collected and then are subjected to centralized treatment.
Preferably, a filter screen is arranged at the gas outlet of the front fraction catcher.
Preferably, the forefraction vacuum pump comprises any one of a water ring vacuum pump, a piston vacuum pump or a roots vacuum pump.
Preferably, the product catcher comprises a product catcher A, a product catcher B and a product vacuum pump which are sequentially connected, and a gas outlet of the product catcher A is connected with a gas inlet of the product catcher B.
Preferably, the raw material supply unit is further provided with a melting catcher connected to the gas outlets of the melting tank and the melting intermediate tank, respectively.
Preferably, the material of the melting catcher comprises carbon steel and/or 304 stainless steel.
Preferably, the outer wall of the melt catcher is provided with a jacket. Water or cold air with the temperature of 40-150 ℃ is introduced into the melting catcher jacket.
Preferably, a baffle is provided within the melt trap, the baffle dividing the front-end trap into two chambers.
Preferably, a filter screen is arranged at the gas outlet of the melting catcher.
Preferably, connecting pipelines among the melting kettle, the pipeline filter, the metering pump, the melting middle tank, the superheater, the rectifying tower, the refining kettle, the condenser and the product receiving kettle are all jacket pipelines. And heat conducting oil is introduced into the jacket pipeline to control the stability of the temperature of the materials in the pipeline.
Preferably, the material of the jacket pipe comprises any one of 304 stainless steel, monel 400 or hastelloy.
In a second aspect, the present invention provides a method for purifying chlorothalonil by using the purifying device according to the first aspect, which is characterized in that the method comprises the following steps:
(1) Melting the chlorothalonil raw material, and heating the melted chlorothalonil to the bubble point;
(2) Rectifying the chlorothalonil heated to the bubble point, refining the rectifying tower bottom product, and capturing the product to obtain the chlorothalonil with the hexachlorobenzene content not more than 10 ppm.
Preferably, the chlorothalonil content in the chlorothalonil material in step (1) is between 90 and 99.5wt.%, for example, 90wt.%, 91wt.%, 92wt.%, 93wt.%, 94wt.%, 95wt.%, 96wt.%, 97wt.%, 98wt.%, 99wt.%, or 99.5wt.%, preferably between 95 and 99wt.%.
Preferably, the hexachlorobenzene content of the chlorothalonil raw material is 10-100ppm, for example, 10ppm, 20ppm, 30ppm, 40ppm, 50ppm, 60ppm, 70ppm, 80ppm, 90ppm or 100ppm, preferably 30-80ppm.
Preferably, the melting temperature is 260-350 ℃, for example 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃ or 350 ℃, preferably 300-330 ℃.
Preferably, the bubble point temperature is 260-350deg.C, such as 260 deg.C, 270 deg.C, 280 deg.C, 290 deg.C, 300 deg.C, 310 deg.C, 320 deg.C, 330 deg.C, 340 deg.C or 350 deg.C, preferably 300-330 deg.C;
preferably, the stripping section temperature of the rectification in step (2) is 300-350deg.C, such as 300 deg.C, 310 deg.C, 320 deg.C, 330 deg.C, 340 deg.C or 350 deg.C, preferably 320-330 deg.C.
Preferably, the temperature of the rectifying section of the rectification is 260-330 ℃, for example 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃ or 330 ℃, preferably 280-300 ℃.
Preferably, the absolute vacuum degree of the top of the rectification column is 0.05-0.095MPa, for example, 0.05MPa, 0.01MPa, 0.02MPa, 0.03MPa, 0.04MPa, 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa or 0.095MPa, preferably 0.06-0.08MPa.
Preferably, the overhead condenser temperature of the rectification is 250-330 ℃, for example 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃ or 330 ℃, preferably 260-290 ℃.
Preferably, the bottom reboiler temperature of the rectification is 300-350 ℃, for example, 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃ or 350 ℃, preferably 310-330 ℃.
Preferably, the temperature of the refining treatment is 260-350deg.C, such as 260-270 deg.C, 280 deg.C, 290 deg.C, 300 deg.C, 310 deg.C, 320 deg.C, 330 deg.C, 340 deg.C or 350 deg.C, preferably 300-330 deg.C.
Preferably, the vacuum degree of the refining treatment is 0.05 to 0.095MPa, for example, 0.05MPa, 0.01MPa, 0.02MPa, 0.03MPa, 0.04MPa, 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa or 0.095MPa, preferably 0.06 to 0.08MPa.
Preferably, the temperature of the trapping is 40-150 ℃, for example 40 ℃, 50 ℃,60 ℃, 70 ℃,80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃, preferably 60-80 ℃.
As a preferred technical solution of the method provided in the second aspect of the present invention, the method includes the following steps:
(1) Melting chlorothalonil material with hexachlorobenzene content of 10-100ppm at 260-350deg.C, and heating to bubble point temperature of 260-350deg.C;
(2) And (3) rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 300-350 ℃, the temperature of a rectifying section is 260-330 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.05-0.095MPa, the temperature of a tower top condenser is 250-330 ℃, the temperature of a tower bottom reboiler is 300-350 ℃, refining the tower bottom product, the refining temperature is 260-350 ℃, the vacuum degree of refining is 0.05-0.095MPa, and the refined product is trapped at 40-150 ℃ to obtain the chlorothalonil product with hexachlorobenzene not exceeding 10 ppm.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the rectifying tower is combined with the refining kettle, and the chlorothalonil with the hexachlorobenzene content of 10-100ppm is refined by using the rectifying kettle after being rectified by the rectifying tower, so that the hexachlorobenzene content in the chlorothalonil product is reduced to be less than 10ppm, the chlorothalonil content in the chlorothalonil product can reach 99.7%, and the purifying device provided by the invention can be used for continuous production and has low operation cost.
Drawings
Fig. 1 is a schematic diagram of a purifying apparatus according to embodiment 2 of the present invention.
Wherein: 1, a raw material bin; 2, a screw conveyor; 3, melting the kettle; 4, a pipeline filter; 5, a plunger metering pump; 6, melting the middle groove; 7, a superheater; 8, a rectifying tower; 9, refining the kettle; 10, a condenser; 11, a product receiving kettle; 12, a melt catcher; 13, a front cut catcher; 14, a product catcher A;15, a product catcher B;16, a front-end vacuum pump; 17, a product vacuum pump. .
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
I) Purification device
Example 1
The embodiment provides a purifying device for producing chlorothalonil with the concentration of hexachlorobenzene not exceeding 10ppm, which comprises a raw material supply unit, a purifying unit and a product collecting unit which are sequentially connected.
The purifying unit comprises a rectifying tower 8, a refining kettle 9 and a condenser 10, wherein a bottom discharge hole of the rectifying tower 8 is connected with a feed inlet of the refining kettle 9, a discharge hole of the refining kettle 9 is connected with a feed inlet of the condenser 10, the rectifying tower 8, the refining kettle 9 and the condenser 10 are made of 304 stainless steel, a heat tracing pipe is arranged on the outer wall of the rectifying tower 8, a tubular condenser 10 is arranged on the top of the rectifying tower 8, a tubular reboiler is arranged at the bottom of the rectifying tower 8, a jacket is arranged on the outer wall of the refining kettle 9, a coil pipe and mechanical stirring are arranged in the kettle of the refining kettle 9, and the condenser 10 is a tubular heat exchanger.
The raw material supply unit comprises a raw material bin 1, a screw conveyor 2, a melting kettle 3, a pipeline filter 4, a plunger type metering pump 5, a melting middle tank 6 and a superheater 7 which are sequentially connected, wherein a discharge hole of the superheater 7 is connected with a feed hole of a rectifying tower 8. The material of former feed bin 1, melting cauldron 3, pipeline filter 4, plunger type measuring pump 5, melting intermediate tank 6 and superheater 7 is 304 stainless steel, the outer wall of melting cauldron 3 is provided with the clamp cover, and the outer wall of melting intermediate tank 6 is provided with the clamp cover, and superheater 7 is tubular heat exchanger.
The product collecting unit comprises a product receiving kettle 11, a product catcher A14, a product catcher B15 and a piston type vacuum pump, wherein a feed inlet of the product receiving kettle 11 is connected with a discharge outlet of the condenser 10, a top steam outlet of the product receiving kettle 11 is connected with a feed inlet of the product catcher, a gas outlet of the product catcher is connected with a product vacuum pump 17, the product receiving kettle 11, the product catcher A14 and the product catcher B15 are made of 304 stainless steel, a jacket is arranged on the outer wall of the product receiving kettle 11, a jacket is arranged on the outer wall of the product catcher A14 and the outer wall of the product catcher B15, and a baffle plate is arranged in the product catcher and divides the product catcher into two chambers.
The connecting pipelines among the melting kettle 3, the pipeline filter 4, the plunger type metering pump 5, the melting middle tank 6, the superheater 7, the rectifying tower 8, the refining kettle 9, the condenser 10 and the product receiving kettle 11 are all jacket pipelines, and the jacket pipelines are made of 304 stainless steel.
The raw materials of the chlorothalonil are continuously conveyed into a melting kettle 3 through a raw material bin 1 and a screw conveyor 2, the raw materials of the chlorothalonil are melted into liquid in the melting kettle 3, impurities are filtered through a pipeline filter 4 and then continuously conveyed into a melting middle tank 6 through a plunger type metering pump 5, the raw materials of the chlorothalonil enter a rectifying tower 8 continuously from the middle part of the rectifying tower 8 after being heated to the bubble point temperature through a superheater 7, light components with higher hexachlorobenzene content are produced from the top of the tower, the chlorothalonil which is preliminarily separated flows into a refining kettle 9 and is evaporated to the gaseous state in the refining kettle 9, the condensed materials flow into a product receiving kettle 11 after being condensed through a condenser 10, and the uncondensed gases are condensed in a product catcher A14 and a product catcher B15, so that solids in the product receiving kettle 11, the product catcher A14 and the product catcher B15 are qualified products.
Example 2
This example provides a purification apparatus for producing chlorothalonil with a hexachlorobenzene content of not more than 10ppm, the schematic diagram of the purification apparatus being shown in fig. 1, the purification apparatus comprising a raw material supply unit, a purification unit and a product collection unit connected in this order.
The purifying unit comprises a rectifying tower 8, a refining kettle 9, a condenser 10, a front fraction catcher 13 and a front fraction vacuum pump 16, wherein a bottom discharge hole of the rectifying tower 8 is connected with a feed hole of the refining kettle 9, a discharge hole of the refining kettle 9 is connected with a feed hole of the condenser 10, the rectifying tower 8, the refining kettle 9, the front fraction catcher 13 and the condenser 10 are made of 304 stainless steel, a heat tracing pipe is arranged on the outer wall of the rectifying tower 8, a tubular condenser 10 is arranged on the top of the rectifying tower 8, a tubular reboiler is arranged at the bottom of the rectifying tower 8, a jacket is arranged on the outer wall of the refining kettle 9, a coil and mechanical stirring are arranged in the kettle of the refining kettle 9, the condenser 10 is a tubular heat exchanger, the front fraction catcher 13 is used for catching light components produced by the rectifying tower 8, the front fraction vacuum pump 16 is connected with a gas outlet of the front fraction catcher 13, a baffle plate is arranged in the front fraction catcher 13, the baffle plate is used for collecting the front fraction catcher 13, and the front fraction is a water-out of the filter screen is a vacuum pump 16 is arranged at the front fraction vacuum pump.
The raw material supply unit comprises a raw material bin 1, a screw conveyor 2, a melting kettle 3, a pipeline filter 4, a plunger type metering pump 5, a melting middle tank 6, a melting catcher 12 and a superheater 7 which are sequentially connected, wherein a discharge port of the superheater 7 is connected with a feed port of a rectifying tower 8. The material of former feed bin 1, melting cauldron 3, pipeline filter 4, plunger metering pump 5, melting intermediate tank 6, melting trap 12 and superheater 7 is 304 stainless steel, the outer wall of melting cauldron 3 is provided with the clamp cover, and the outer wall of melting intermediate tank 6 is provided with the clamp cover, and superheater 7 is tubular heat exchanger, and the outer wall of melting trap 12 is provided with the clamp cover, is provided with the baffle in the melting trap 12, the baffle divide into two rooms with melting trap 12, the gas outlet department of melting trap 12 is provided with the filter screen.
The product collecting unit comprises a product receiving kettle 11, a product catcher A14, a product catcher B15 and a product vacuum pump 17, wherein a feed inlet of the product receiving kettle 11 is connected with a discharge outlet of the condenser 10, a top steam outlet of the product receiving kettle 11 is connected with a feed inlet of the product catcher A14, a gas outlet of the product catcher is connected with the product vacuum pump 17, materials of the product receiving kettle 11, the product catcher A14 and the product catcher B15 are 304 stainless steel, a jacket is arranged on the outer wall of the product receiving kettle 11, a jacket is arranged on the outer wall of the product catcher A14 and the outer wall of the product catcher B15, and a baffle plate is arranged in the product catcher and divides the product catcher into two chambers.
The connecting pipelines among the melting kettle 3, the pipeline filter 4, the plunger type metering pump 5, the melting middle tank 6, the superheater 7, the rectifying tower 8, the refining kettle 9, the condenser 10 and the product receiving kettle 11 are all jacket pipelines, and the jacket pipelines are made of 304 stainless steel.
The raw materials of the chlorothalonil are continuously conveyed into a melting kettle 3 through a raw material bin 1 and a screw conveyor 2, the raw materials of the chlorothalonil are melted into liquid in the melting kettle 3, impurities are filtered through a pipeline filter 4 and then continuously conveyed into a melting middle tank 6 through a plunger type metering pump 5, the raw materials of the chlorothalonil enter a rectifying tower 8 continuously from the middle part of the rectifying tower 8 after being heated to the bubble point temperature through a superheater 7, light components with higher hexachlorobenzene content are produced from the top of the tower, the chlorothalonil which is preliminarily separated flows into a refining kettle 9 and is evaporated to the gaseous state in the refining kettle 9, the condensed materials flow into a product receiving kettle 11 after being condensed through a condenser 10, and the uncondensed gases are condensed in a product catcher A14 and a product catcher B15, so that solids in the product receiving kettle 11, the product catcher A14 and the product catcher B15 are qualified products.
The gas generated in the melting kettle 3 enters a melting catcher 12, and the solid powder in the melting catcher 12 can be used as chlorothalonil raw material to return to the raw material bin 1; the gas produced at the top of the rectifying tower 8 enters a front cut catcher 13, and solid powder in the front cut catcher 13 is solid waste and is concentrated and then treated as solid waste.
Comparative example 1
The comparative example provides a purification device of chlorothalonil, and compared with the embodiment 1, the purification unit provided by the comparative example is not provided with a refining kettle, and the bottom product of the rectifying tower is directly converted into a solid product in a product collecting kettle after flowing through a condenser.
II) purification method
Application example 1
The present application example provides a method for purifying a chlorothalonil raw material using the purification apparatus of example 2, the method comprising the steps of:
(1) Melting a chlorothalonil raw material with the hexachlorobenzene content of 60ppm at 300 ℃, and heating to the bubble point temperature, wherein the chlorothalonil content in the chlorothalonil raw material is 95wt.%;
(2) And rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 330 ℃, the temperature of a rectifying section is 300 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.08MPa, the temperature of a condenser at the top of the rectifying tower is 290 ℃, the temperature of a reboiler at the bottom of the rectifying tower is 330 ℃, the refining treatment temperature of the bottom product is 330 ℃, the absolute vacuum degree of the refining treatment is 0.07MPa, and the refined product is trapped at 80 ℃ to obtain the chlorothalonil product with the hexachlorobenzene of 6 ppm.
Application example 2
The present application example provides a method for purifying a chlorothalonil raw material using the purification apparatus of example 2, the method comprising the steps of:
(1) Melting a chlorothalonil raw material with the hexachlorobenzene content of 40ppm at the temperature of 280 ℃, and heating to the bubble point temperature, wherein the chlorothalonil content in the chlorothalonil raw material is 92wt.%;
(2) And rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 320 ℃, the temperature of a rectifying section is 280 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.06MPa, the temperature of a condenser at the top of the rectifying tower is 260 ℃, the temperature of a reboiler at the bottom of the rectifying tower is 310 ℃, the refining treatment temperature of the bottom product is 300 ℃, the absolute vacuum degree of the refining treatment is 0.06MPa, and the refined product is trapped at 60 ℃ to obtain the chlorothalonil product with the concentration of 5ppm of hexachlorobenzene.
Application example 3
The present application example provides a method for purifying a chlorothalonil raw material using the purification apparatus of example 2, the method comprising the steps of:
(1) Melting a chlorothalonil raw material with the hexachlorobenzene content of 100ppm at 350 ℃, and heating to the bubble point temperature, wherein the chlorothalonil content in the chlorothalonil raw material is 99wt.%;
(2) And rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 350 ℃, the temperature of a rectifying section is 330 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.095MPa, the temperature of a condenser at the top of the rectifying tower is 330 ℃, the temperature of a reboiler at the bottom of the rectifying tower is 350 ℃, refining the bottom product, the refining temperature is 350 ℃, the absolute vacuum degree of the refining is 0.05MPa, and the refined product is trapped at 150 ℃ to obtain the chlorothalonil product with the hexachlorobenzene of 10 ppm.
Application example 4
The present application example provides a method for purifying a chlorothalonil raw material using the purification apparatus of example 2, the method comprising the steps of:
(1) Melting a chlorothalonil raw material with the hexachlorobenzene content of 10ppm at 260 ℃ and heating to the bubble point temperature, wherein the chlorothalonil content in the chlorothalonil raw material is 90wt.%;
(2) And rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 300 ℃, the temperature of a rectifying section is 260 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.05MPa, the temperature of a condenser at the top of the rectifying tower is 250 ℃, the temperature of a reboiler at the bottom of the rectifying tower is 300 ℃, the refining treatment temperature of the bottom product is 260 ℃, the absolute vacuum degree of the refining treatment is 0.095MPa, and the refined product is trapped at 40 ℃ to obtain the chlorothalonil product with the concentration of 2ppm of hexachlorobenzene.
Application example 5
The present application example provides a method for purifying a chlorothalonil raw material using the purification apparatus of example 1, the method comprising the steps of:
(1) Melting a chlorothalonil raw material with the hexachlorobenzene content of 60ppm at 300 ℃, and heating to the bubble point temperature, wherein the chlorothalonil content in the chlorothalonil raw material is 95wt.%;
(2) And rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 330 ℃, the temperature of a rectifying section is 300 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.08MPa, the temperature of a condenser at the top of the rectifying tower is 290 ℃, the temperature of a reboiler at the bottom of the rectifying tower is 330 ℃, the refining treatment temperature of the bottom product is 330 ℃, the absolute vacuum degree of the refining treatment is 0.07MPa, and the refined product is trapped at 80 ℃ to obtain the chlorothalonil product with the hexachlorobenzene of 6 ppm.
Comparative example 1 was used
The present comparative application provides a method for purifying chlorothalonil raw material using the purifying apparatus of comparative example 1, the method comprising the steps of:
(1) Melting a chlorothalonil raw material with the hexachlorobenzene content of 60ppm at 300 ℃, and heating to the bubble point temperature, wherein the chlorothalonil content in the chlorothalonil raw material is 95wt.%;
(2) And rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 330 ℃, the temperature of a rectifying section is 300 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.08MPa, the temperature of a condenser at the top of the rectifying tower is 290 ℃, the temperature of a reboiler at the bottom of the rectifying tower is 330 ℃, and the product at the bottom of the rectifying tower is cooled at 80 ℃ to obtain a chlorothalonil product with the concentration of hexachlorobenzene of 15ppm.
The invention provides application examples 1-5 and application comparative example 1, wherein the raw material of chlorothalonil is treated, and the obtained chlorothalonil product and the recovery rate of the chlorothalonil are analyzed, and the analysis results are shown in table 1:
TABLE 1
As can be seen from application examples 1-4, the purification method provided by the invention is used for purifying the chlorothalonil raw material, the content of the chlorothalonil in the purified chlorothalonil product is 99.4-99.7wt%, the content of hexachlorobenzene is 2-10ppm, and the recovery rate of the chlorothalonil is 98.1-98.9wt%.
The purification device used in application example 5 is provided by example 1, and a melting catcher is not arranged in example 1, so that the raw material of the chlorothalonil entrained by the melting tail gas cannot be recovered, and therefore, the recovery rate of the chlorothalonil in application example 5 is 96.8wt% and is lower than that of the chlorothalonil in application example 1 by 98.6wt%.
The purification device used in comparative application example 1 is provided by comparative example 1, a refining kettle is not arranged in comparative example 1, the chlorothalonil product is obtained after the rectifying tower bottom product is cooled, and the chlorothalonil content in the chlorothalonil product is reduced from 99.6wt% to 99.2% and the hexachlorobenzene content is increased from 6ppm to 15ppm because the rectifying tower bottom product is not subjected to refining treatment of the refining tower.
In conclusion, the invention combines the rectifying tower with the refining kettle, and the chlorothalonil with the hexachlorobenzene content of 10-100ppm is refined by using the rectifying kettle after being rectified by the rectifying tower, so that the hexachlorobenzene content in the chlorothalonil product is reduced to be less than 10ppm, the chlorothalonil content in the chlorothalonil product can reach 99.7 percent, and the purifying device provided by the invention can be used for continuous production and has low operation cost.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (65)
1. A purifying device for producing chlorothalonil with the concentration of hexachlorobenzene not more than 10ppm, which is characterized by comprising a raw material supply unit, a purifying unit and a product collecting unit which are connected in sequence;
the purifying unit comprises a rectifying tower, a refining kettle and a condenser, wherein a bottom discharge hole of the rectifying tower is connected with a feed inlet of the refining kettle, and a discharge hole of the refining kettle is connected with a feed inlet of the condenser;
the raw material supply unit comprises a raw material bin, a raw material conveying device, a melting kettle, a pipeline filter, a metering pump, a melting middle tank and a superheater which are sequentially connected, wherein a discharge port of the superheater is connected with a feed port of the rectifying tower;
the product collecting unit comprises a product receiving kettle, a product catcher and a product vacuum pump, wherein a feed inlet of the product receiving kettle is connected with a discharge outlet of the condenser, a top steam outlet of the product receiving kettle is connected with a feed inlet of the product catcher, and a gas outlet of the product catcher is connected with the product vacuum pump;
the raw material supply unit is also provided with a melting catcher which is respectively connected with the gas outlets of the melting kettle and the melting middle tank.
2. The purifying apparatus of claim 1, wherein the rectifying column is made of any one of 304 stainless steel, monel 400, and hastelloy.
3. The purifying apparatus according to claim 1, wherein the rectifying column outer wall is provided with a heat tracing pipe.
4. The purifying apparatus according to claim 1, wherein a column tube type condenser is provided at the top of the rectifying column.
5. The purification device according to claim 1, wherein a shell and tube reboiler is provided at the bottom of the rectifying column.
6. The purifying apparatus of claim 1, wherein the material of the purifying kettle comprises any one of 304 stainless steel, monel 400, and hastelloy.
7. The purifying apparatus according to claim 1, wherein an outer wall of the refining vessel is provided with a jacket.
8. The purifying apparatus according to claim 1, wherein a coil is provided in the refining vessel.
9. The purification apparatus according to claim 1, wherein the refining tank is provided with mechanical agitation.
10. The purification apparatus of claim 1, wherein the condenser comprises any one of 304 stainless steel, monel 400, or hastelloy.
11. The purification apparatus of claim 1, wherein the condenser is a shell and tube heat exchanger.
12. The purifying device according to claim 1, wherein the material of the raw stock bin comprises carbon steel and/or 304 stainless steel.
13. Purification device according to claim 1, characterized in that the raw material conveying means comprise a conveyor belt and/or a screw conveyor.
14. The purifying apparatus of claim 1, wherein the melting vessel comprises any one of 304 stainless steel, monel 400, or hastelloy.
15. The purifying apparatus according to claim 1, wherein an outer wall of the melting tank is provided with a jacket.
16. The purification apparatus of claim 1, wherein the tubing filter comprises any one of 304 stainless steel, monel 400, or hastelloy.
17. The purification apparatus of claim 1, wherein the molten intermediate tank comprises any one of 304 stainless steel, monel 400, or hastelloy.
18. The purification apparatus according to claim 1, wherein the outer wall of the melting intermediate tank is provided with a jacket.
19. The purification apparatus of claim 1, wherein the superheater comprises any one of 304 stainless steel, monel 400, or hastelloy.
20. The purification apparatus of claim 1, wherein the superheater is a tube array heat exchanger.
21. The purification apparatus of claim 1, wherein the metering pump comprises any one of 304 stainless steel, monel 400, or hastelloy.
22. Purification device according to claim 1, characterized in that the metering pump comprises a plunger metering pump and/or a diaphragm metering pump.
23. The purification apparatus of claim 1, wherein the product receiving vessel comprises any one of 304 stainless steel, monel 400, or hastelloy.
24. The purification apparatus according to claim 1, wherein the outer wall of the product receiving tank is provided with a jacket.
25. The purification apparatus of claim 1, wherein the product catcher comprises carbon steel and/or 304 stainless steel.
26. The purification device according to claim 1, wherein the outer wall of the product catcher is provided with a jacket.
27. The purifying apparatus of claim 1, wherein a baffle is disposed within the product trap, the baffle dividing the product trap into two chambers.
28. The purification apparatus of claim 1, wherein the product vacuum pump comprises any one of a water ring vacuum pump, a piston vacuum pump, or a roots vacuum pump.
29. The purification apparatus of claim 1, wherein the purification unit is further provided with a front-end trap for trapping light components produced at the top of the rectifying column and a front-end vacuum pump connected to a gas outlet of the front-end trap.
30. The purification apparatus of claim 29, wherein the front-end trap material comprises carbon steel and/or 304 stainless steel.
31. The purification apparatus of claim 29, wherein the outer wall of the front end trap is provided with a jacket.
32. The purification apparatus of claim 29, wherein a baffle is disposed within the front-end trap, the baffle dividing the front-end trap into two chambers.
33. The purification apparatus of claim 29, wherein a filter screen is provided at the gas outlet of the front end trap.
34. The purification apparatus of claim 29, wherein the forecut vacuum pump comprises any one or a combination of two or more of a water ring vacuum pump, a piston vacuum pump, or a roots vacuum pump.
35. The purifying device of claim 1, wherein the product trap comprises a product trap a, a product trap B and a product vacuum pump connected in sequence, and a gas outlet of the product trap a is connected with a gas inlet of the product trap B.
36. The purification apparatus of claim 1, wherein the product vacuum pump comprises any one or a combination of two or more of a water ring vacuum pump, a piston vacuum pump, or a roots vacuum pump.
37. The purification apparatus of claim 1, wherein the material of the melt catcher comprises carbon steel and/or 304 stainless steel.
38. The purification apparatus of claim 1, wherein the outer wall of the melt catcher is provided with a jacket.
39. The purification apparatus of claim 1, wherein a baffle is disposed within the melt catcher, the baffle dividing the melt catcher into two chambers.
40. The purification apparatus of claim 1, wherein a filter screen is provided at a gas outlet of the melt catcher.
41. The purification apparatus of claim 1, wherein the connecting lines between the melting tank, the pipe filter, the metering pump, the melting intermediate tank, the superheater, the rectifying column, the refining tank, the condenser, and the product receiving tank are all jacketed pipes.
42. The purification apparatus of claim 41, wherein the jacketed piping comprises any one of 304 stainless steel, monel 400, or hastelloy.
43. A method of purifying chlorothalonil using the purification apparatus of any one of claims 1-42, the method comprising the steps of:
(1) Melting the chlorothalonil raw material, and heating the melted chlorothalonil to the bubble point; the content of hexachlorobenzene in the chlorothalonil raw material is 10-100ppm;
(2) Rectifying the chlorothalonil heated to the bubble point, refining the bottom product of the rectifying tower, and capturing the product to obtain chlorothalonil with the hexachlorobenzene content of not more than 10 ppm;
the temperature of the refining treatment is 260-350 ℃, and the vacuum degree of the refining treatment is 0.05-0.095MPa.
44. The method of claim 43, wherein the chlorothalonil material in step (1) has a chlorothalonil content of between 90 and 99.5wt.%.
45. The method of claim 44, wherein the chlorothalonil material in step (1) has a chlorothalonil content of between 95 and 99wt.%.
46. The method of claim 43, wherein the chlorothalonil material has a hexachlorobenzene content of between 30 and 80ppm.
47. The method of claim 43, wherein the melting temperature is 260-350 ℃.
48. The method of claim 43, wherein the melting temperature is 300-330 ℃.
49. The method of claim 43, wherein the bubble point temperature is 260-350 ℃.
50. The method of claim 49, wherein the bubble point temperature is 300-330 ℃.
51. The process of claim 43 wherein the stripping section temperature of said rectifying in step (2) is 300-350 ℃.
52. The method of claim 51 wherein the stripping section temperature of the rectifying of step (2) is 320-330 ℃.
53. The method of claim 43, wherein the temperature of the rectifying section of the rectification is 260-330 ℃.
54. The method of claim 53, wherein the temperature of the rectifying section of the rectification is 280 ℃ to 300 ℃.
55. The method of claim 43, wherein the absolute vacuum at the top of the rectification column is from 0.05 to 0.095MPa.
56. The method of claim 55, wherein the absolute vacuum at the top of the rectification column is from 0.06MPa to 0.08MPa.
57. The method of claim 43, wherein the overhead condenser temperature of the rectification is 250-330 ℃.
58. The method of claim 57, wherein the overhead condenser temperature of the rectification is from 260 ℃ to 290 ℃.
59. The method of claim 43, wherein the bottoms reboiler temperature of the rectification is 300 to 350 ℃.
60. The method of claim 59, wherein the bottoms reboiler temperature of the rectification is from 310 ℃ to 330 ℃.
61. The method of claim 43, wherein the temperature of the refining treatment is 300-330 ℃.
62. The method according to claim 43, wherein the vacuum degree of the refining treatment is 0.06 to 0.08MPa.
63. The method of claim 43, wherein the trapped temperature is 40-150 ℃.
64. The method of claim 63, wherein the temperature of trapping is 60-80 ℃.
65. The method of claim 43, wherein the method comprises the steps of:
(1) Melting chlorothalonil raw material with hexachlorobenzene content of 10-100ppm at 260-350 ℃, and heating to bubble point temperature of 260-350 ℃, wherein the chlorothalonil content in the chlorothalonil raw material is 90-99.5 wt%;
(2) And (3) rectifying the chlorothalonil heated to the bubble point, wherein the temperature of a stripping section is 300-350 ℃, the temperature of a rectifying section is 260-330 ℃, the absolute vacuum degree of the top of the rectifying tower is 0.05-0.095MPa, the temperature of a tower top condenser is 250-330 ℃, the temperature of a tower bottom reboiler is 300-350 ℃, refining the tower bottom product, the refining temperature is 260-350 ℃, the vacuum degree of refining is 0.05-0.095MPa, and the refined product is trapped at 40-150 ℃ to obtain the chlorothalonil product with hexachlorobenzene not exceeding 10 ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811486502.4A CN109293529B (en) | 2018-12-06 | 2018-12-06 | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811486502.4A CN109293529B (en) | 2018-12-06 | 2018-12-06 | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109293529A CN109293529A (en) | 2019-02-01 |
| CN109293529B true CN109293529B (en) | 2023-11-24 |
Family
ID=65142716
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811486502.4A Active CN109293529B (en) | 2018-12-06 | 2018-12-06 | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109293529B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001213856A (en) * | 2000-01-28 | 2001-08-07 | Msk Management Kk | Method of purification for 2,4,5,6-tetrachloro-1,3- benzenedicarbonitrile |
| CN1948278A (en) * | 2006-11-07 | 2007-04-18 | 云南省化工研究院 | Production method of low hexachlorobenzene content chlorothalonil |
| CN104447407A (en) * | 2014-12-08 | 2015-03-25 | 江阴苏利化学股份有限公司 | Method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm |
| CN107056650A (en) * | 2016-10-20 | 2017-08-18 | 江苏维尤纳特精细化工有限公司 | The preparation of high-purity Bravo |
| CN207576343U (en) * | 2017-11-18 | 2018-07-06 | 江阴苏利化学股份有限公司 | A kind of low content Bravo refining plant |
| CN108329235A (en) * | 2018-03-02 | 2018-07-27 | 天津赛普泰克科技有限公司 | A kind of process producing high-purity Bravo |
-
2018
- 2018-12-06 CN CN201811486502.4A patent/CN109293529B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001213856A (en) * | 2000-01-28 | 2001-08-07 | Msk Management Kk | Method of purification for 2,4,5,6-tetrachloro-1,3- benzenedicarbonitrile |
| CN1948278A (en) * | 2006-11-07 | 2007-04-18 | 云南省化工研究院 | Production method of low hexachlorobenzene content chlorothalonil |
| CN104447407A (en) * | 2014-12-08 | 2015-03-25 | 江阴苏利化学股份有限公司 | Method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm |
| CN107056650A (en) * | 2016-10-20 | 2017-08-18 | 江苏维尤纳特精细化工有限公司 | The preparation of high-purity Bravo |
| CN207576343U (en) * | 2017-11-18 | 2018-07-06 | 江阴苏利化学股份有限公司 | A kind of low content Bravo refining plant |
| CN108329235A (en) * | 2018-03-02 | 2018-07-27 | 天津赛普泰克科技有限公司 | A kind of process producing high-purity Bravo |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109293529A (en) | 2019-02-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110845366B (en) | Preparation method and preparation system of chlorothalonil | |
| CN104815447A (en) | DMAC (dimethylacetamide) or DMF (dimethyl formamide) waste liquid four-tower double-effect rectification system and recovery method thereof | |
| CN108329235B (en) | Process for producing high-purity chlorothalonil | |
| CN109265365B (en) | Continuous rectification and purification process for high-content chlorothalonil | |
| CN109052462A (en) | Crude titanic chloride purification removes vanadium method | |
| CN109293529B (en) | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm | |
| CN109231635B (en) | Wastewater treatment process | |
| CN109052463A (en) | A kind of purification of crude titanic chloride removes vanadium method | |
| CN111285783B (en) | Refining and purifying system and method for high-content chlorothalonil | |
| CN209352805U (en) | A kind of purifying plant producing Bravo of the hexachloro-benzene no more than 10ppm | |
| CN209481517U (en) | A kind of unqualified Bravo continuous rectification purification system | |
| CN111285784B (en) | Unqualified chlorothalonil purification system and method | |
| CN109369454B (en) | Continuous rectification and purification system and method for unqualified chlorothalonil | |
| CN207596753U (en) | A kind of production equipment of trichloro-acetic chloride | |
| CN109438284B (en) | Continuous rectification purification process for low-content chlorothalonil | |
| CN104844420A (en) | Continuous treatment process and device of neopentyl glycol condensed washing mother liquor | |
| CN109821265A (en) | A kind of thick raffinate rectifier unit of caprolactam and technique | |
| CN113480461B (en) | Method for continuously synthesizing perchloromethyl mercaptan by utilizing reaction tower | |
| WO2019061593A1 (en) | Method for extracting high-purity ethoxyquinoline by using multistage molecular distillation technology | |
| CN210394218U (en) | Separation device for recovering chloroethylene and 1, 1-dichloroethane from chloroethylene high-boiling residues | |
| CN107382758A (en) | A kind of method that glycine is reclaimed in the concentrating spent liquor from glycine | |
| CN110590604A (en) | Continuous rectification and purification device for m-phthalonitrile | |
| CN210796292U (en) | Continuous rectification and purification device for m-phthalonitrile | |
| CN219922095U (en) | Refining purification multistage distillation tower | |
| CN213589738U (en) | Solvent S-270 purification device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |