CN111870988B - Trapping method and trapping system for tetrachloroisophthalonitrile reaction gas - Google Patents
Trapping method and trapping system for tetrachloroisophthalonitrile reaction gas Download PDFInfo
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- CN111870988B CN111870988B CN202010694307.1A CN202010694307A CN111870988B CN 111870988 B CN111870988 B CN 111870988B CN 202010694307 A CN202010694307 A CN 202010694307A CN 111870988 B CN111870988 B CN 111870988B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- 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
Abstract
The invention provides a method and a system for trapping tetrachloroisophthalonitrile reaction gas, wherein the trapping method comprises the following steps: and filtering the reaction gas conveyed by the upstream production line, then feeding the reaction gas into a multistage trapping unit, mixing the reaction gas with liquid nitrogen at least twice in the multistage trapping unit, and sublimating the reaction gas after mixing with the liquid nitrogen to trap and separate out tetrachloroisophthalonitrile in the reaction gas. According to the invention, liquid nitrogen is used as a cooling medium of the trapping device, the liquid nitrogen enters the trapping device through the distributor to be directly vaporized, tetrachloroisophthalonitrile gas in reaction gas is contacted with the liquid nitrogen to be directly desublimated and separated out to the bottom of the trapping device, and the tetrachloroisophthalonitrile gas enters the product bin through the conveyor, so that the traditional air cooling or water cooling mode is replaced by liquid nitrogen cooling, the phenomena of material wall formation and material collapse caused by cooling of the reaction gas by using a jacket cooling medium in the traditional trapping process are effectively avoided, and the technical problem that the normal production is influenced due to the blockage of a discharge port at the bottom of the trapping device is effectively solved.
Description
Technical Field
The invention belongs to the technical field of product trapping, relates to a trapping method and a trapping system, and particularly relates to a trapping method and a trapping system for tetrachloroisophthalonitrile reaction gas.
Background
Tetrachloroisophthalonitrile, also called chlorothalonil, is a high-efficiency, low-toxicity and broad-spectrum protective bactericide which is mainly used for preventing and treating various fungal diseases, and the action mechanism of the tetrachloroisophthalonitrile is that the tetrachloroisophthalonitrile can act with glyceraldehyde triphosphate dehydrogenase in fungal cells and is combined with protein containing cysteine in the enzyme, so that the activity of the enzyme is damaged, and the metabolism of the fungal cells is damaged to lose the vitality. Chlorothalonil has no internal absorption and conduction effects, but has good adhesion on the body surface after being sprayed on plants, and is not easy to be washed away by rainwater, so the pesticide effect period is longer. Is mainly used for preventing and treating rust disease, anthracnose, powdery mildew and downy mildew on fruit trees and vegetables. The bactericidal composition is mainly used for preventing rust disease, anthracnose, powdery mildew and downy mildew on fruit trees and vegetables and preventing plants from being damaged by fungi. Tetrachloroisophthalonitrile is also used abroad for sterilization of golf courses, lawns and ornamental plants, and for preservative treatment of some trees and paintings.
The simplest and most economical manufacturing process of tetrachloroisophthalonitrile is as follows: the isophthalonitrile is melted and then sent into a vaporizer to be vaporized or directly atomized with a part of gas flow through a nozzle to be subjected to a reactor. Chlorine gas is mixed with gaseous isophthalonitrile after being dried and preheated, and nitrogen is used as diluent gas for vaporization or atomization of isophthalonitrile and adjustment of reactant concentration. The reactor adopts a fluidized bed or other forms, gas after reaction enters a catcher, chlorothalonil is desublimated and separated out and is continuously sent out to obtain the product, and the yield is 90%. The tail gas is mainly chlorine, hydrogen chloride and nitrogen, and can be partially circulated or completely removed from a tail gas recovery treatment system. Liquid carbon tetrachloride can be sprayed into the catcher, and after the liquid carbon tetrachloride is contacted with the reaction gas, chlorothalonil is sublimated and separated out. The carbon tetrachloride is vaporized and discharged together with the tail gas, and is further cooled to-6 ℃, and the carbon tetrachloride is condensed for recycling.
The indirect cooling type trapping is also called square box type trapping, and is a commonly used trapping mode for domestic small tetrachloroisophthalonitrile manufacturers at present. The mixed reaction gas out of the fluidized bed reactor enters a fixed bed for further reaction after being filtered by a filter, then enters a people square box type trap through a jacket heat-conducting oil heat-preserving pipe, the trap is provided with an outer jacket and cools the mixed reaction gas through circulating cooling water, a crystallized material is desublimated and freely settled in the trap, tetrachloroisophthalonitrile is conveyed to a crushing device through a product conveying system, and a finished product tetrachloroisophthalonitrile is obtained after crushing. Because the desublimation and crystallization process of tetrachloroisophthalonitrile is not a constant temperature process, and the trapping of all materials cannot be completed in one trap generally, the operation needs to be carried out in a mode of connecting a plurality of square boxes in series. At present, the most used plants are operated in series by boxes until the content of the tetrachloroisophthalonitrile remaining in the mixed reaction gas reaches the lower economic limit of recovery. The induced draft fan is established to the tail gas processing apparatus export, guarantees that whole entrapment system can not lead to revealing of poisonous and harmful reaction gas during the ejection of compact at little negative pressure state.
However, most of the existing trapping devices adopt air cooling or water cooling as a cooling medium, and the cooling medium needs to flow in a jacket, so that the blocking of a discharge port at the bottom of the trapping device due to the phenomena of material wall bonding and material collapse is easily caused, and the normal trapping operation is influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a trapping method and a trapping system for tetrachloroisophthalonitrile reaction gas, wherein liquid nitrogen is used as a cooling medium of a trapping device, the liquid nitrogen enters the trapping device through a distributor to be directly vaporized, the tetrachloroisophthalonitrile gas in the reaction gas is contacted with the liquid nitrogen to be directly desublimated and separated out tetrachloroisophthalonitrile to the bottom of the trapping device, and the tetrachloroisophthalonitrile gas enters a product bin through a conveyor, the traditional air-cooling or water-cooling indirect trapping mode is replaced by the liquid nitrogen direct-contact trapping, so that the phenomena of wall bonding and material collapse caused by cooling, crystallization and separation of the reaction gas on the inner wall of the trapping device due to small heat exchange area and large local temperature difference of a jacket cooling medium used in the traditional trapping process are effectively avoided, thereby effectively solving the technical problem that the discharge hole at the bottom of the trapping device is blocked to influence the normal production.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for capturing tetrachloroisophthalonitrile reaction gas, the method comprising:
and filtering the reaction gas conveyed by the upstream production line, then feeding the reaction gas into a multistage trapping unit, mixing the reaction gas with liquid nitrogen at least twice in the multistage trapping unit, and sublimating the reaction gas after mixing with the liquid nitrogen to trap and separate out tetrachloroisophthalonitrile in the reaction gas.
According to the invention, liquid nitrogen is used as a cooling medium of the trapping device, the liquid nitrogen enters the trapping device through the distributor to be directly vaporized, tetrachloroisophthalonitrile gas in reaction gas is contacted with the liquid nitrogen to be directly desublimated and separated out to the bottom of the trapping device, and the tetrachloroisophthalonitrile gas enters the product bin through the conveyor, so that the traditional air cooling or water cooling mode is replaced by liquid nitrogen cooling, the phenomena of material wall formation and material collapse caused by cooling of the reaction gas by using a jacket cooling medium in the traditional trapping process are effectively avoided, and the technical problem that the normal production is influenced due to the blockage of a discharge port at the bottom of the trapping device is effectively solved.
According to the invention, liquid nitrogen is directly introduced into the trapping device and directly contacts with the reaction gas, so that the contact heat exchange area of the reaction gas and a heat exchange medium is remarkably increased compared with that of the traditional jacket type trapping process, meanwhile, the multistage trapping process is matched, the unqualified solid waste amount is reduced to a certain extent, and the trapping efficiency and the production benefit are greatly improved.
As a preferred embodiment of the present invention, the trapping method specifically includes:
reaction gas conveyed by an upstream production line is filtered by a bag type filtering device and then is introduced into a fixed bed filtering device through a heat preservation pipe;
(II) the reaction gas discharged by the fixed bed filtering device sequentially flows through a first trapping device and a second trapping device, is respectively mixed with liquid nitrogen in the first trapping device and the second trapping device, and is desublimated after being mixed with the liquid nitrogen, and tetrachloroisophthalonitrile separated out of the reaction gas is trapped;
(III) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, wherein the filtered tail gas is divided into two parts, one part is recycled to the first trapping device, and the other part is discharged after tail gas treatment.
As a preferable technical scheme, in the step (I), a jacket is arranged on the outer side of the heat preservation pipe, and a heat-conducting medium is introduced into the jacket.
Preferably, the heat conducting medium is heat conducting oil.
Preferably, the heat transfer oil is low-temperature heat transfer oil, medium-temperature heat transfer oil or high-temperature heat transfer oil, and further preferably, the heat transfer oil is high-temperature heat transfer oil.
Preferably, the temperature of the heat-conducting medium is 330 to 350 ℃, for example, 330 ℃, 331 ℃, 332 ℃, 333 ℃, 334 ℃, 335 ℃, 336 ℃, 337 ℃, 338 ℃, 339 ℃, 340 ℃, 341 ℃, 342 ℃, 343 ℃, 344 ℃, 345 ℃, 346 ℃, 347 ℃, 348 ℃, 349 ℃ or 350 ℃, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the temperature in the heat preservation pipe is controlled by adjusting the temperature of the heat conducting medium in the jacket.
Preferably, automatic interlocking control is carried out between the temperature in the heat preservation pipe and the flow of the heat-conducting medium.
Preferably, the flow rate of the heat-conducting medium is 20-30 m3H, for example, may be 20m3/h、21m3/h、22m3/h、23m3/h、24m3/h、25m3/h、26m3/h、27m3/h、28m3/h、29m3H or 30m3H, further preferably, the flow rate of the heat-conducting medium is 25m3And/h, but not limited to, the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the temperature in the heat-insulating tube is controlled to 320 to 340 ℃, for example, 320 ℃, 321 ℃, 322 ℃, 323 ℃, 324 ℃, 325 ℃, 326 ℃, 327 ℃, 328 ℃, 329 ℃, 330 ℃, 331 ℃, 332 ℃, 333 ℃, 334 ℃, 335 ℃, 336 ℃, 337 ℃, 338 ℃, 339 ℃ or 340 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the step (II), the liquid nitrogen is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device.
Preferably, the trapping temperatures in the first trapping device and the second trapping device are respectively controlled by independently adjusting the flow rates of liquid nitrogen.
Preferably, automatic interlocking control is carried out between the trapping temperature and the liquid nitrogen flow rate in the first trapping device and the second trapping device.
Preferably, the liquid nitrogen is introduced into the first capturing device at a flow rate of 75 to 200kg/h, for example, 75kg/h, 80kg/h, 85kg/h, 90kg/h, 95kg/h, 100kg/h, 105kg/h, 110kg/h, 115kg/h, 120kg/h, 125kg/h, 130kg/h, 135kg/h, 140kg/h, 145kg/h, 150kg/h, 155kg/h, 160kg/h, 165kg/h, 170kg/h, 175kg/h, 180kg/h, 185kg/h, 190kg/h, 195kg/h or 200kg/h, but not limited to the values listed, and other values not listed in this range are equally applicable.
Preferably, the collection temperature in the first collection device is controlled to 140 to 180 ℃, for example, 140 ℃, 142 ℃, 144 ℃, 146 ℃, 148 ℃, 150 ℃, 152 ℃, 154 ℃, 156 ℃, 158 ℃, 160 ℃, 162 ℃, 164 ℃, 168 ℃, 170 ℃, 172 ℃, 174 ℃, 176 ℃, 178 ℃ or 180 ℃, and more preferably, the collection temperature in the first collection device is controlled to 150 to 170 ℃, but is not limited to the values listed, and other values not listed within the range of values are also applicable.
Preferably, the flow rate of the liquid nitrogen introduced into the second trap device is 20 to 45kg/h, and may be, for example, 20kg/h, 21kg/h, 22kg/h, 23kg/h, 24kg/h, 25kg/h, 26kg/h, 27kg/h, 28kg/h, 29kg/h, 30kg/h, 31kg/h, 32kg/h, 33kg/h, 34kg/h, 35kg/h, 36kg/h, 37kg/h, 38kg/h, 39kg/h, 40kg/h, 41kg/h, 42kg/h, 43kg/h, 44kg/h or 45kg/h, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the collection temperature in the second collection device is controlled to be 100 to 140 ℃, for example, 100 ℃, 102 ℃, 104 ℃, 106 ℃, 108 ℃, 110 ℃, 112 ℃, 114 ℃, 116 ℃, 118 ℃, 120 ℃, 122 ℃, 124 ℃, 126 ℃, 128 ℃, 130 ℃, 132 ℃, 134 ℃, 136 ℃, 138 ℃ or 140 ℃, and more preferably, the collection temperature in the second collection device is 110 to 130 ℃, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the first trapping device has a trapping efficiency of 70 to 90%, for example, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, or 90%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
Preferably, the second capturing device has a capturing efficiency of 5 to 25%, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24% or 25%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
Preferably, the liquid nitrogen content is 99 to 99.9%, for example, 99.0%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, or 99.9%, and more preferably, the liquid nitrogen content is 99.9%, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the tetrachloroisophthalonitrile captured by the first capture device and the tetrachloroisophthalonitrile captured by the second capture device are respectively led into a product conveying system.
In a preferred technical scheme of the present invention, in the step (iii), a jacket is arranged outside the tail gas filtering device, and a cooling medium is introduced into the jacket.
Preferably, the cooling medium is circulating water or frozen brine, and further preferably, the cooling medium is circulating water.
Preferably, the temperature of the cooling medium is 10 to 20 ℃, for example, 10 ℃, 11 ℃, 12 ℃, 13 ℃, 14 ℃, 15 ℃, 16 ℃, 17 ℃, 18 ℃, 19 ℃ or 20 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the temperature within the exhaust gas filtering device is controlled by adjusting the flow rate of the cooling medium within the jacket.
Preferably, the automatic interlocking control is carried out between the temperature in the tail gas filtering device and the flow of the cooling medium.
Preferably, the flow of the cooling medium is 10-15 m3H, for example, may be 10m3/h、11m3/h、12m3/h、13m3/h、14m3H or 15m3And/h, but not limited to, the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the temperature in the exhaust gas filtering device is controlled to be 50 to 80 ℃, for example, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃, 60 ℃, 62 ℃, 64 ℃, 66 ℃, 68 ℃, 70 ℃, 72 ℃, 74 ℃, 76 ℃, 78 ℃ or 80 ℃, and more preferably, the temperature of the exhaust gas filtering device is controlled to be 60 to 70 ℃, but the temperature is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the tail gas discharged from the second capturing device is filtered by a tail gas filtering device to remove solid waste therein, and the tail gas after being filtered to remove solid waste is divided into a first tail gas and a second tail gas according to a volume ratio, wherein the volume ratio of the first tail gas to the second tail gas is 0.11-0.25, for example, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.20, 0.21, 0.22, 0.23, 0.24 or 0.25, but not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
Preferably, the first tail gas is returned to the first trapping device through a fan, and the cold energy in the first tail gas is circularly applied in the first trapping device.
In the invention, the tail gas filtered by the tail gas filtering device returns to the first capturing device through the fan, thereby effectively utilizing the cold energy of the tail gas and greatly reducing the loss of liquid nitrogen.
Preferably, the air volume of the fan is 150-300 m3H, for example, may be 150m3/h、160m3/h、170m3/h、180m3/h、190m3/h、200m3/h、210m3/h、220m3/h、230m3/h、240m3/h、250m3/h、260m3/h、270m3/h、280m3/h、290m3H or 300m3H, further preferably, the air volume of the fan is 300m3And/h, but not limited to, the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the second tail gas is treated by the tail gas treatment device and then is led out by the exhaust fan for emission.
Preferably, the flow of the exhaust fan is 5000-10000 m3H may be, for example, 5000m3/h、5500m3/h、6000m3/h、6500m3/h、7000m3/h、7500m3/h、8000m3/h、8500m3/h、9000m3/h、9500m3H or 10000m3H, further preferably, the flow of the exhaust fan is 10000m3And/h, but not limited to, the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the wind pressure of the exhaust fan is 1000 to 2500Pa, for example, 1000Pa, 1100Pa, 1200Pa, 1300Pa, 1400Pa, 1500Pa, 1600Pa, 1700Pa, 1800Pa, 1900Pa, 2000Pa, 2100Pa, 2200Pa, 2300Pa, 2400Pa or 2500Pa, and further preferably, the wind pressure of the exhaust fan is 2000Pa, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
In a second aspect, the present invention provides a capturing system for tetrachloroisophthalonitrile reaction gas, the capturing system being used for carrying out the capturing method of the first aspect, the capturing system comprising a filtration unit and a multistage capturing unit which are connected.
The multistage trapping unit comprises at least two trapping devices which are connected in sequence, and the trapping devices are respectively connected with a liquid nitrogen supply device.
As a preferable technical solution of the present invention, the filtration unit includes a bag filtration device and a fixed bed filtration device connected in sequence.
Preferably, the bag type filtering device and the fixed bed filtering device are connected through a heat preservation pipe.
Preferably, the outer side of the heat preservation pipe is provided with a jacket, and a heat-conducting medium is introduced into the jacket.
Preferably, the heat conducting medium is heat conducting oil.
Preferably, a reaction gas temperature sensor is arranged in the heat preservation pipe, a heat-conducting medium flow control valve is arranged on a jacket liquid inlet pipeline of the heat preservation pipe, the reaction gas temperature sensor is connected with the reaction gas flow control valve in a feedback mode, and the opening degree of the heat-conducting medium flow control valve is controlled in real time through the reaction gas temperature in the pipe detected by the reaction gas temperature sensor.
As a preferable technical solution of the present invention, the air inlet of the trapping device is provided with a uniform distribution device.
Preferably, the product outlets of the trapping devices are respectively connected with a product conveying system.
Preferably, the multistage trapping unit comprises a first trapping device and a second trapping device which are connected in sequence, and the first trapping device and the second trapping device are respectively connected with a liquid nitrogen supply device.
Preferably, a first electric control valve is arranged on a connecting pipeline between the first trapping device and the liquid nitrogen supply device, and a second electric control valve is arranged on a connecting pipeline between the first trapping device and the liquid nitrogen supply device.
Preferably, a first temperature sensing device and a second temperature sensing device are respectively arranged in the first trapping device and the second trapping device, the first temperature sensing device is connected with the first electric control valve in a feedback mode, and the second temperature sensing device is connected with the second electric control valve in a feedback mode.
As a preferable technical scheme, the trapping system further comprises a tail gas filtering device and a tail gas treatment device which are sequentially connected with the outlets of the multistage trapping units.
Preferably, the outer side of the tail gas filtering device is provided with a jacket, and a cooling medium is introduced into the jacket.
Preferably, the cooling medium is circulating water or frozen brine, and further preferably, the cooling medium is circulating water.
Preferably, a tail gas temperature sensor is arranged in the tail gas filtering device, a cooling medium flow control valve is arranged on a jacket liquid inlet pipeline of the tail gas filtering device, the tail gas temperature sensor is connected with the cooling medium flow control valve in a feedback mode, and the opening degree of the cooling medium flow control valve is controlled in real time through the tail gas temperature detected by the tail gas temperature sensor.
Preferably, the tail gas outlet of the tail gas filtering device is divided into two paths, one path is connected with the first trapping device in a returning mode, and the other path is connected with a downstream tail gas treatment device.
In a preferred embodiment of the present invention, a fan is disposed on the connection pipeline between the tail gas filtering device and the first trapping device.
Preferably, the material of the fan is steel lining PTFE or glass fiber reinforced plastic, and further preferably, the material of the fan is glass fiber reinforced plastic.
Preferably, the exhaust port of the tail gas treatment device is provided with an induced draft fan.
The system refers to an equipment system, or a production equipment.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, liquid nitrogen is used as a cooling medium of the trapping device, the liquid nitrogen enters the trapping device through the distributor to be directly vaporized, tetrachloroisophthalonitrile gas in reaction gas is contacted with the liquid nitrogen to be directly desublimated and separated out to the bottom of the trapping device, and the tetrachloroisophthalonitrile gas enters the product bin through the conveyor, so that the traditional air cooling or water cooling mode is replaced by liquid nitrogen cooling, the phenomena of material wall formation and material collapse caused by cooling of the reaction gas by using a jacket cooling medium in the traditional trapping process are effectively avoided, and the technical problem that the normal production is influenced due to the blockage of a discharge port at the bottom of the trapping device is effectively solved.
(2) According to the invention, liquid nitrogen is directly introduced into the trapping device and directly contacts with the reaction gas, so that the contact heat exchange area of the reaction gas and a heat exchange medium is remarkably increased compared with that of the traditional jacket type trapping process, meanwhile, the multistage trapping process is matched, the unqualified solid waste amount is reduced to a certain extent, and the trapping efficiency and the production benefit are greatly improved.
(3) The tail gas part filtered by the tail gas filtering device returns to the catching device through the fan, thereby effectively utilizing the cold energy of the tail gas and greatly reducing the loss of liquid nitrogen.
Drawings
Fig. 1 is a block diagram of a system according to an embodiment of the present invention.
Detailed Description
It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be taken as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
It should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "disposed," "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
In one embodiment, the invention provides a capture system for tetrachloroisophthalonitrile reaction gas, which is shown in figure 1 and comprises a filtering unit and a multi-stage capture unit which are connected.
The filtering unit comprises a bag type filtering device and a fixed bed filtering device which are connected in sequence. The bag type filtering device is connected with the fixed bed filtering device through a heat preservation pipe, a jacket is arranged on the outer side of the heat preservation pipe, a heat conducting medium is introduced into the jacket, and the heat conducting medium is heat conducting oil. The reaction temperature sensor is arranged in the heat preservation pipe, the heat-conducting medium flow control valve is arranged on the jacket liquid inlet pipeline of the heat preservation pipe, the reaction temperature sensor is connected with the reaction gas flow control valve in a feedback mode, and the opening degree of the heat-conducting medium flow control valve is controlled in real time through the reaction gas temperature in the pipe detected by the reaction gas temperature sensor.
The multistage trapping unit comprises at least two trapping devices which are connected in sequence, and the trapping devices are respectively connected with a liquid nitrogen supply device. The air inlet of the trapping device is provided with a uniform distribution device, and the product outlets of the trapping device are respectively connected with a product conveying system. In the present embodiment, the multistage trapping unit includes a first trapping device and a second trapping device connected in sequence, and the first trapping device and the second trapping device are connected to a liquid nitrogen supply device, respectively. A first electric control valve is arranged on a connecting pipeline of the first trapping device and the liquid nitrogen supply device, and a second electric control valve is arranged on a connecting pipeline of the first trapping device and the liquid nitrogen supply device. And a first temperature sensing device and a second temperature sensing device are respectively arranged in the first trapping device and the second trapping device, the first temperature sensing device is connected with the first electric control valve in a feedback manner, and the second temperature sensing device is connected with the second electric control valve in a feedback manner.
The trapping system also comprises a tail gas filtering device and a tail gas processing device which are sequentially connected with the outlets of the multistage trapping units. The outer side of the tail gas filtering device is provided with a jacket, and a cooling medium is introduced into the jacket and can be selected from circulating water or frozen brine. Be provided with tail gas temperature sensor in the tail gas filter equipment, be provided with cooling medium flow control valve on tail gas filter equipment's the cover feed liquor pipeline, tail gas temperature sensor and cooling medium flow control valve feedback are connected, the tail gas temperature real-time control cooling medium flow control valve's that detects through tail gas temperature sensor aperture. The tail gas outlet of the tail gas filtering device is divided into two paths, one path is connected with the first trapping device in a loop mode, and the other path is connected with the downstream tail gas treatment device. And a fan is arranged on a connecting pipeline between the tail gas filtering device and the first trapping device, and the material of the fan can be steel lining PTFE or glass fiber reinforced plastic. And an induced draft fan is arranged at an exhaust port of the tail gas treatment device.
In another embodiment, the present invention provides a method for capturing tetrachloroisophthalonitrile reaction gas, the method comprising:
(1) reaction gas conveyed by the upstream production line is filtered by the bag type filtering device and then is introduced into the fixed bed filtering device through the heat preservation pipe. Introducing a heat-conducting medium into a jacket of the heat-insulating pipe, and heating reaction gas flowing through the heat-insulating pipe, wherein the temperature of the heat-conducting medium is 330-350 ℃; the temperature in the heat-insulating pipe is controlled by adjusting the flow of the heat-conducting medium in the jacket, and the flow of the heat-conducting medium is 20-30 m3The temperature in the heat preservation pipe is controlled to be 320-340 ℃;
(2) the method comprises the following steps that reaction gas discharged by a fixed bed filtering device sequentially flows through a first trapping device and a second trapping device, liquid nitrogen with the content of 99-99.9% is respectively and independently introduced into the first trapping device and the second trapping device through a uniform distribution device, the reaction gas is respectively mixed with the liquid nitrogen in the first trapping device and the second trapping device, the reaction gas is mixed with the liquid nitrogen and then desublimated, tetrachloroisophthalonitrile separated out of the reaction gas is trapped and introduced into a product conveying system;
the method comprises the following steps of respectively controlling the trapping temperature in a first trapping device and the trapping temperature in a second trapping device by independently adjusting the flow of liquid nitrogen, wherein the flow of the liquid nitrogen introduced into the first trapping device is 75-200 kg/h, and the trapping temperature in the first trapping device is controlled at 140-180 ℃; the flow of liquid nitrogen introduced into the second trapping device is 20-45 kg/h, and the trapping temperature in the second trapping device is controlled to be 100-140 ℃; the collecting efficiency of the first collecting device is 70-90%, and the collecting efficiency of the second collecting device is 5-25%;
(3) the tail gas discharged by the second trapping device is introduced into a tail gas filtering device, the tail gas entering the tail gas filtering device is cooled by a cooling medium in a jacket of the tail gas filtering device, the cooling medium is circulating water or frozen salt water, the temperature of the cooling medium is 10-20 ℃, the temperature of the cooling medium in the tail gas filtering device is controlled by adjusting the flow of the cooling medium in the jacket, and the flow of the cooling medium is 10-15 m3The temperature in the tail gas filtering device is controlled to be 50-80 ℃;
the tail gas filtering device filters solid waste in the tail gas, tail gas after solid waste filtering is divided into first tail gas and second tail gas according to volume ratio, and the first tail gas and the second tail gas areThe volume ratio of the tail gas is 0.11-0.25, the first tail gas is returned to the first trapping device through the fan, the cold quantity in the first tail gas is circularly applied to the first trapping device, and the air quantity of the fan is 150-300 m3H; the second tail gas is treated by a tail gas treatment device and then is led out and discharged by an exhaust fan, and the flow of the exhaust fan is 5000-10000 m3And h, the air pressure of the exhaust fan is 1000-2500 Pa.
Example 1
The embodiment provides a method for trapping tetrachloroisophthalonitrile reaction gas, which comprises the following steps:
(1) reaction gas conveyed by the upstream production line is filtered by the bag type filtering device and then is introduced into the fixed bed filtering device through the heat preservation pipe. Introducing a heat-conducting medium into a jacket of the heat-insulating pipe, and heating the reaction gas flowing through the heat-insulating pipe, wherein the temperature of the heat-conducting medium is 330 ℃; the temperature in the heat-insulating pipe is controlled by adjusting the flow of the heat-conducting medium in the jacket, and the flow of the heat-conducting medium is 30m3The temperature in the heat preservation pipe is controlled to be 320 ℃;
(2) reaction gas discharged by the fixed bed filtering device sequentially flows through the first trapping device and the second trapping device, liquid nitrogen with the content of 99% is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device, the reaction gas is respectively mixed with the liquid nitrogen in the first trapping device and the second trapping device, the reaction gas is mixed with the liquid nitrogen and then desublimated, tetrachloroisophthalonitrile separated out in the reaction gas is trapped and introduced into a product conveying system respectively;
the trapping temperature in the first trapping device and the trapping temperature in the second trapping device are respectively controlled by independently adjusting the flow of liquid nitrogen, the flow of the liquid nitrogen introduced into the first trapping device is 75kg/h, and the trapping temperature in the first trapping device is controlled at 140 ℃; the flow of liquid nitrogen introduced into the second trapping device is 45kg/h, and the trapping temperature in the second trapping device is controlled at 140 ℃;
(3) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, cooling the tail gas entering the tail gas filtering device by a cooling medium in a jacket of the tail gas filtering device, wherein the cooling medium is circulating water or frozen brine, the temperature of the cooling medium is 10 ℃, and adjusting the temperatureThe flow rate of the whole cooling medium in the jacket controls the temperature in the tail gas filtering device, and the flow rate of the cooling medium is 10m3The temperature in the tail gas filtering device is controlled at 50 ℃;
the tail gas filtering device filters solid waste in the tail gas, the tail gas after solid waste filtering is divided into a first tail gas and a second tail gas according to the volume ratio, the volume ratio of the first tail gas to the second tail gas is 0.11, the first tail gas is returned to the first collecting device through the fan, cold energy in the first tail gas is circularly applied to the first collecting device, and the air volume of the fan is 150m3H; the second tail gas is treated by a tail gas treatment device and then is led out and discharged by an exhaust fan, and the flow rate of the exhaust fan is 5000m3And h, the air pressure of the exhaust fan is 1000 Pa.
By the above-mentioned trapping method, the trapping rate of the first trapping device was 70%, the trapping rate of the second trapping device was 25%, and the total trapping rate of tetrachloroisophthalonitrile was 95%.
Example 2
The embodiment provides a method for trapping tetrachloroisophthalonitrile reaction gas, which comprises the following steps:
(1) reaction gas conveyed by the upstream production line is filtered by the bag type filtering device and then is introduced into the fixed bed filtering device through the heat preservation pipe. Introducing a heat-conducting medium into a jacket of the heat-insulating pipe, and heating the reaction gas flowing through the heat-insulating pipe, wherein the temperature of the heat-conducting medium is 335 ℃; the temperature in the heat-conducting medium in the flow control heat-insulating pipe in the jacket is adjusted, and the flow of the heat-conducting medium is 27m3The temperature in the heat preservation pipe is controlled at 325 ℃;
(2) reaction gas discharged by the fixed bed filtering device sequentially flows through the first trapping device and the second trapping device, liquid nitrogen with the content of 99.2% is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device, the reaction gas is respectively mixed with the liquid nitrogen in the first trapping device and the second trapping device, the reaction gas is mixed with the liquid nitrogen and then desublimated, tetrachloroisophthalonitrile separated out of the reaction gas is trapped and is respectively introduced into the product conveying system;
the trapping temperature in the first trapping device and the trapping temperature in the second trapping device are respectively controlled by independently adjusting the flow of liquid nitrogen, the flow of the liquid nitrogen introduced into the first trapping device is 100kg/h, and the trapping temperature in the first trapping device is controlled at 150 ℃; the flow of liquid nitrogen introduced into the second trapping device is 40kg/h, and the trapping temperature in the second trapping device is controlled at 130 ℃;
(3) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, cooling the tail gas entering the tail gas filtering device by using a cooling medium in a jacket of the tail gas filtering device, wherein the cooling medium is circulating water or frozen brine, the temperature of the cooling medium is 13 ℃, controlling the temperature in the tail gas filtering device by adjusting the flow of the cooling medium in the jacket, and the flow of the cooling medium is 14m3The temperature in the tail gas filtering device is controlled at 60 ℃;
the tail gas filtering device filters solid waste in the tail gas, the tail gas after solid waste filtering is divided into first tail gas and second tail gas according to the volume ratio, the volume ratio of the first tail gas to the second tail gas is 0.15, the first tail gas is returned to the first collecting device through the fan, cold energy in the first tail gas is circularly applied to the first collecting device, and the air volume of the fan is 180m3H; the second tail gas is treated by a tail gas treatment device and then is led out and discharged by an exhaust fan, and the flow rate of the exhaust fan is 6000m3And h, the air pressure of the exhaust fan is 1500 Pa.
By the above-mentioned trapping method, the trapping rate of the first trapping device was 75%, the trapping rate of the second trapping device was 23%, and the total trapping rate of tetrachloroisophthalonitrile reached 98%.
Example 3
The embodiment provides a method for trapping tetrachloroisophthalonitrile reaction gas, which comprises the following steps:
(1) reaction gas conveyed by the upstream production line is filtered by the bag type filtering device and then is introduced into the fixed bed filtering device through the heat preservation pipe. Introducing a heat-conducting medium into a jacket of the heat-insulating pipe, and heating the reaction gas flowing through the heat-insulating pipe, wherein the temperature of the heat-conducting medium is 340 ℃; the temperature in the heat-insulating pipe is controlled by adjusting the flow of the heat-conducting medium in the jacket, and the flow of the heat-conducting medium is 25m3The temperature in the heat preservation pipe is controlled to be 330 ℃;
(2) reaction gas discharged by the fixed bed filtering device sequentially flows through the first trapping device and the second trapping device, liquid nitrogen with the content of 99.5 percent is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device, the reaction gas is respectively mixed with the liquid nitrogen in the first trapping device and the second trapping device, the reaction gas is mixed with the liquid nitrogen and then desublimated, tetrachloroisophthalonitrile separated out of the reaction gas is trapped and is respectively introduced into the product conveying system;
the trapping temperature in the first trapping device and the trapping temperature in the second trapping device are respectively controlled by independently adjusting the flow of liquid nitrogen, the flow of the liquid nitrogen introduced into the first trapping device is 135kg/h, and the trapping temperature in the first trapping device is controlled at 160 ℃; the flow of liquid nitrogen introduced into the second trapping device is 30kg/h, and the trapping temperature in the second trapping device is controlled at 120 ℃;
(3) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, cooling the tail gas entering the tail gas filtering device by using a cooling medium in a jacket of the tail gas filtering device, wherein the cooling medium is circulating water or frozen brine, the temperature of the cooling medium is 15 ℃, controlling the temperature in the tail gas filtering device by adjusting the flow of the cooling medium in the jacket, and the flow of the cooling medium is 12m3The temperature in the tail gas filtering device is controlled at 70 ℃;
the tail gas filtering device filters solid waste in the tail gas, the tail gas after solid waste filtering is divided into a first tail gas and a second tail gas according to the volume ratio, the volume ratio of the first tail gas to the second tail gas is 0.18, the first tail gas is returned to the first collecting device through the fan, cold energy in the first tail gas is circularly used in the first collecting device, and the air volume of the fan is 200m3H; the second tail gas is treated by the tail gas treatment device and then is led out and discharged by an exhaust fan, and the flow rate of the exhaust fan is 8000m3And h, the air pressure of the exhaust fan is 1800 Pa.
By the above-mentioned trapping method, the trapping rate of the first trapping device was 80%, the trapping rate of the second trapping device was 16%, and the total trapping rate of tetrachloroisophthalonitrile was 96%.
Example 4
The embodiment provides a method for trapping tetrachloroisophthalonitrile reaction gas, which comprises the following steps:
(1) reaction gas conveyed by the upstream production line is filtered by the bag type filtering device and then is introduced into the fixed bed filtering device through the heat preservation pipe. Introducing a heat-conducting medium into a jacket of the heat-insulating pipe, and heating the reaction gas flowing through the heat-insulating pipe, wherein the temperature of the heat-conducting medium is 345 ℃; the temperature in the heat-insulating pipe is controlled by adjusting the flow of the heat-conducting medium in the jacket, and the flow of the heat-conducting medium is 23m3The temperature in the heat preservation pipe is controlled at 335 ℃;
(2) reaction gas discharged by the fixed bed filtering device sequentially flows through the first trapping device and the second trapping device, liquid nitrogen with the content of 99.7% is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device, the reaction gas is respectively mixed with the liquid nitrogen in the first trapping device and the second trapping device, the reaction gas is mixed with the liquid nitrogen and then desublimated, tetrachloroisophthalonitrile separated out of the reaction gas is trapped and is respectively introduced into the product conveying system;
the trapping temperature in the first trapping device and the trapping temperature in the second trapping device are respectively controlled by independently adjusting the flow of liquid nitrogen, the flow of the liquid nitrogen introduced into the first trapping device is 170kg/h, and the trapping temperature in the first trapping device is controlled at 170 ℃; the flow of liquid nitrogen introduced into the second trapping device is 25kg/h, and the trapping temperature in the second trapping device is controlled at 110 ℃;
(3) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, cooling the tail gas entering the tail gas filtering device by using a cooling medium in a jacket of the tail gas filtering device, wherein the cooling medium is circulating water or frozen brine, the temperature of the cooling medium is 17 ℃, controlling the temperature in the tail gas filtering device by adjusting the flow of the cooling medium in the jacket, and the flow of the cooling medium is 11m3The temperature in the tail gas filtering device is controlled to be 75 ℃;
the tail gas filtering device filters solid waste in the tail gas, the tail gas after solid waste filtering is divided into a first tail gas and a second tail gas according to the volume ratio, the volume ratio of the first tail gas to the second tail gas is 0.2, the first tail gas is returned to the first collecting device through the fan, cold energy in the first tail gas is circularly applied to the first collecting device, and the air volume of the fan is 250m3H; the second tail gas is treated by a tail gas treatment device and then is led out and discharged by an exhaust fan, and the flow rate of the exhaust fan is 9000m3And h, the air pressure of the exhaust fan is 2000 Pa.
By the above-mentioned trapping method, the trapping rate of the first trapping device was 85%, the trapping rate of the second trapping device was 12%, and the total trapping rate of tetrachloroisophthalonitrile reached 97%.
Example 5
The embodiment provides a method for trapping tetrachloroisophthalonitrile reaction gas, which comprises the following steps:
(1) reaction gas conveyed by the upstream production line is filtered by the bag type filtering device and then is introduced into the fixed bed filtering device through the heat preservation pipe. Introducing a heat-conducting medium into a jacket of the heat-insulating pipe, and heating the reaction gas flowing through the heat-insulating pipe, wherein the temperature of the heat-conducting medium is 350 ℃; the temperature in the heat-insulating pipe is controlled by adjusting the flow of the heat-conducting medium in the jacket, and the flow of the heat-conducting medium is 20m3The temperature in the heat preservation pipe is controlled to be 340 ℃;
(2) reaction gas discharged by the fixed bed filtering device sequentially flows through the first trapping device and the second trapping device, liquid nitrogen with the content of 99.9 percent is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device, the reaction gas is respectively mixed with the liquid nitrogen in the first trapping device and the second trapping device, the reaction gas is mixed with the liquid nitrogen and then desublimated, tetrachloroisophthalonitrile separated out of the reaction gas is trapped and is respectively introduced into the product conveying system;
the trapping temperature in the first trapping device and the trapping temperature in the second trapping device are respectively controlled by independently adjusting the flow of liquid nitrogen, the flow of the liquid nitrogen introduced into the first trapping device is 200kg/h, and the trapping temperature in the first trapping device is controlled at 180 ℃; the flow of liquid nitrogen introduced into the second trapping device is 20kg/h, and the trapping temperature in the second trapping device is controlled at 100 ℃;
(3) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, cooling the tail gas entering the tail gas filtering device by a cooling medium in a jacket of the tail gas filtering device, wherein the cooling medium is circulating water or frozen brine, the temperature of the cooling medium is 20 ℃, and introducing the tail gas into a pipelineThe temperature in the tail gas filtering device is controlled by adjusting the flow rate of the cooling medium in the jacket, and the flow rate of the cooling medium is 10m3The temperature in the tail gas filtering device is controlled to be 80 ℃;
the tail gas filtering device filters solid waste in the tail gas, the tail gas after solid waste filtering is divided into a first tail gas and a second tail gas according to the volume ratio, the volume ratio of the first tail gas to the second tail gas is 0.25, the first tail gas is returned to the first collecting device through the fan, cold energy in the first tail gas is circularly applied to the first collecting device, and the air volume of the fan is 300m3H; the second tail gas is treated by a tail gas treatment device and then is led out and discharged by an exhaust fan, and the flow of the exhaust fan is 10000m3And h, the air pressure of the exhaust fan is 2500 Pa.
By the above-mentioned trapping method, the trapping rate of the first trapping device was 90%, the trapping rate of the second trapping device was 5%, and the total trapping rate of tetrachloroisophthalonitrile was 95%.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (52)
1. A method for collecting tetrachloroisophthalonitrile reaction gas, which is characterized by comprising the following steps:
reaction gas conveyed by an upstream production line is filtered by a bag type filtering device and then is introduced into a fixed bed filtering device through a heat preservation pipe;
(II) the reaction gas discharged by the fixed bed filtering device sequentially flows through a first trapping device and a second trapping device, is respectively mixed with liquid nitrogen in the first trapping device and the second trapping device, and is desublimated after being mixed with the liquid nitrogen, and tetrachloroisophthalonitrile separated out of the reaction gas is trapped;
liquid nitrogen is respectively and independently introduced into the first trapping device and the second trapping device through the uniform distribution device; the trapping temperatures in the first trapping device and the second trapping device are respectively controlled by independently adjusting the flow of liquid nitrogen; the content of the liquid nitrogen is 99-99.9%; the trapping temperature in the first trapping device is controlled to be 168-180 ℃; the trapping temperature in the second trapping device is controlled to be 110-130 ℃;
(III) introducing the tail gas discharged by the second trapping device into a tail gas filtering device, wherein the filtered tail gas is divided into two parts, one part is recycled to the first trapping device, and the other part is discharged after tail gas treatment.
2. The capturing method according to claim 1, wherein in step (I), the outer side of the heat preservation pipe is provided with a jacket, and a heat-conducting medium is introduced into the jacket.
3. The capturing method according to claim 2, characterized in that the heat transfer medium is a heat transfer oil.
4. The capture method according to claim 3, wherein the thermal oil is a low temperature thermal oil, a medium temperature thermal oil, or a high temperature thermal oil.
5. The capturing method according to claim 4, wherein the thermal oil is a high temperature thermal oil.
6. The capturing method according to claim 2, wherein the temperature of the heat transfer medium is 330 to 350 ℃.
7. The capture method of claim 2, wherein the temperature in the holding tube is controlled by adjusting the temperature of the heat transfer medium in the jacket.
8. The capturing method according to claim 7, wherein automatic interlock control is performed between the temperature in the heat-retaining pipe and the flow rate of the heat transfer medium.
9. The trapping method of claim 2, which isCharacterized in that the flow of the heat-conducting medium is 20-30 m3/h。
10. The capturing method according to claim 9, wherein the flow rate of the heat transfer medium is 25m3/h。
11. The capturing method according to claim 2, characterized in that the temperature in the heat-insulating pipe is controlled to 320-340 ℃.
12. The capturing method according to claim 1, characterized in that automatic interlocking control is performed between the capturing temperature and the flow rate of liquid nitrogen in the first capturing device and the second capturing device.
13. The capturing method according to claim 1, wherein the flow rate of liquid nitrogen introduced into the first capturing device is 75 to 200 kg/h.
14. The capture method according to claim 1, wherein the flow rate of the liquid nitrogen introduced into the second capture device is 20 to 45 kg/h.
15. The capturing method according to claim 1, wherein the capturing efficiency of the first capturing device is 70 to 90%.
16. The capturing method according to claim 1, wherein the capturing efficiency of the second capturing device is 5 to 25%.
17. The capture method according to claim 1, characterized in that the liquid nitrogen content is 99.9%.
18. The capturing method according to claim 1, wherein tetrachloroisophthalonitrile captured by the first capturing device and the second capturing device is separately introduced into a product conveying system.
19. The capturing method according to claim 1, wherein in the step (iii), a jacket is provided outside the off-gas filtering device, and a cooling medium is introduced into the jacket.
20. The capture method of claim 19, wherein the cooling medium is circulating water or chilled brine.
21. The method according to claim 20, wherein the cooling medium is circulating water.
22. The collection method according to claim 19, wherein the temperature of the cooling medium is 10 to 20 ℃.
23. The method of trapping according to claim 19, wherein the temperature within the exhaust gas filtering device is controlled by adjusting the flow rate of the cooling medium within the jacket.
24. The method according to claim 23, wherein automatic interlocking control is performed between the temperature in the exhaust gas filtering device and the flow rate of the cooling medium.
25. The collection method according to claim 19, wherein the flow rate of the cooling medium is 10 to 15m3/h。
26. The collection method according to claim 19, wherein the temperature in the exhaust gas filtration device is controlled to 50 to 80 ℃.
27. The collection method according to claim 26, wherein the temperature of the exhaust gas filtering device is controlled to be 60 to 70 ℃.
28. The capturing method according to claim 1, wherein the tail gas discharged from the second capturing device is filtered to remove solid waste therein by a tail gas filtering device, the tail gas after being filtered to remove the solid waste is divided into a first tail gas and a second tail gas according to a volume ratio, and the volume ratio of the first tail gas to the second tail gas is 0.11-0.25.
29. The capture method of claim 28, wherein the first exhaust gas is returned to the first capture device by a fan, and the cold in the first exhaust gas is recycled in the first capture device.
30. The collection method according to claim 29, wherein the fan has an air volume of 150 to 300m3/h。
31. The method according to claim 30, wherein the fan has a volume of 300m3/h。
32. The capture method of claim 28, wherein the second exhaust gas is treated by an exhaust gas treatment device and then exhausted by an exhaust fan.
33. The collection method according to claim 32, wherein the flow rate of the exhaust fan is 5000 to 10000m3/h。
34. The capturing method as claimed in claim 33, wherein the flow rate of the exhaust fan is 10000m3/h。
35. The collection method according to claim 32, wherein the exhaust fan has a wind pressure of 1000 to 2500 Pa.
36. The collection method according to claim 35, wherein the exhaust fan has a wind pressure of 2000 Pa.
37. A capturing system for tetrachloroisophthalonitrile reaction gas, characterized in that the capturing system is used for carrying out the capturing method according to any one of claims 1 to 36, and comprises a filtration unit and a multistage capturing unit which are connected;
the multistage trapping unit comprises at least two trapping devices which are connected in sequence, and the trapping devices are respectively connected with a liquid nitrogen supply device.
38. The capture system of claim 37, wherein the filtration unit comprises a bag filtration unit and a fixed bed filtration unit connected in series.
39. The capture system of claim 38, wherein the bag filter unit and the fixed bed filter unit are connected by a thermal insulation pipe.
40. The capture system of claim 39, wherein a reaction gas temperature sensor is arranged in the heat preservation pipe, a heat-conducting medium flow control valve is arranged on a jacket liquid inlet pipeline of the heat preservation pipe, the reaction gas temperature sensor is connected with the reaction gas flow control valve in a feedback mode, and the opening degree of the heat-conducting medium flow control valve is controlled in real time through the reaction gas temperature in the pipe detected by the reaction gas temperature sensor.
41. The trapping system of claim 37, wherein the air inlet of the trapping device is provided with a uniform distribution device.
42. The trapping system of claim 37, wherein the product outlets of the trapping devices are each connected to a product delivery system.
43. The capture system of claim 37, wherein the multi-stage capture unit comprises a first capture device and a second capture device connected in series, and the first capture device and the second capture device are respectively connected with a liquid nitrogen supply device.
44. The trap system according to claim 43, wherein a first electrically controlled valve is provided on a connection pipe between the first trap device and the liquid nitrogen supply device, and a second electrically controlled valve is provided on a connection pipe between the first trap device and the liquid nitrogen supply device.
45. The trapping system according to claim 43, wherein the first trapping device and the second trapping device are each provided with a first temperature sensing device and a second temperature sensing device, the first temperature sensing device is in feedback connection with the first electrically controlled valve, and the second temperature sensing device is in feedback connection with the second electrically controlled valve.
46. The capture system of claim 43, further comprising an exhaust gas filtering device and an exhaust gas treatment device connected in series with the outlet of the multi-stage capture unit.
47. The capture system of claim 46, wherein a tail gas temperature sensor is arranged in the tail gas filtering device, a cooling medium flow control valve is arranged on a jacket liquid inlet pipeline of the tail gas filtering device, the tail gas temperature sensor is connected with the cooling medium flow control valve in a feedback mode, and the opening degree of the cooling medium flow control valve is controlled in real time through the tail gas temperature detected by the tail gas temperature sensor.
48. The capture system of claim 46, wherein the tail gas outlet of the tail gas filtering device is divided into two paths, one path is connected back to the first capture device, and the other path is connected to a downstream tail gas treatment device.
49. The capture system of claim 46, wherein a fan is arranged on the connecting pipeline between the tail gas filtering device and the first capture device.
50. The capture system of claim 49, wherein the blower is steel lined PTFE or FRP.
51. The capture system of claim 50, wherein the blower is made of glass fiber reinforced plastic.
52. The capture system of claim 46, wherein the exhaust port of the tail gas treatment device is provided with an induced draft fan.
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Family Cites Families (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1006043B (en) * | 1985-04-01 | 1989-12-13 | 云南省化工研究所 | Technology of preparation and regeneration of catalyst for the chlorination process of production of tetrachloro-m-benqenedicyanide |
| CN100368387C (en) * | 2006-04-18 | 2008-02-13 | 江阴市苏利精细化工有限公司 | Continuous production method for tetrachloro terephthalonitrile |
| CN201825895U (en) * | 2010-10-14 | 2011-05-11 | 蒙健 | Novel chlorothalonil production device |
| CN102070519B (en) * | 2010-12-06 | 2012-10-10 | 横店集团东阳英洛华绿色电化学有限公司 | Method for purifying 3,4,5,6-tetrachloro-2-cyanopyridine by sublimation and catching, and catcher and system thereof |
| CN102336761A (en) * | 2010-12-17 | 2012-02-01 | 常熟市联邦化工有限公司 | Method for capturing and purifying pyromellitic dianhydride |
| CN103011083A (en) * | 2012-12-04 | 2013-04-03 | 瓮福（集团）有限责任公司 | Gas-phase iodine crystallization method |
| CN204684714U (en) * | 2015-06-04 | 2015-10-07 | 宜昌恒友化工有限公司 | A kind of capturing device of sublimating for penta chloropyridine |
| CN205084758U (en) * | 2015-09-29 | 2016-03-16 | 金堆城钼业股份有限公司 | Many media condensing equipment |
| CN106995387B (en) * | 2016-01-25 | 2020-04-17 | 上海泰禾国际贸易有限公司 | Dry trapping process for isophthalonitrile and/or terephthalonitrile |
| CN205586600U (en) * | 2016-04-13 | 2016-09-21 | 上海泰禾国际贸易有限公司 | A trap for a benzene dicarbonitrile production line |
| CN107513026B (en) * | 2016-06-15 | 2020-02-11 | 江苏新河农用化工有限公司 | Automatic discharging process for dry-method catching of isophthalonitrile |
| 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 |
| CN206746024U (en) * | 2017-01-17 | 2017-12-15 | 上海泰禾国际贸易有限公司 | A kind of trap for para-Phthalonitrile production line |
| CN108212135A (en) * | 2017-12-29 | 2018-06-29 | 南通泰禾化工股份有限公司 | The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology |
| CN108373454B (en) * | 2018-04-08 | 2023-07-25 | 山东鸿运工程设计有限公司 | Melamine production device and production process |
| CN111285783B (en) * | 2018-12-06 | 2023-04-18 | 江苏新河农用化工有限公司 | Refining and purifying system and method for high-content chlorothalonil |
| CN109265365B (en) * | 2018-12-06 | 2021-11-19 | 江苏新河农用化工有限公司 | Continuous rectification and purification process for high-content chlorothalonil |
| CN110280088A (en) * | 2019-06-28 | 2019-09-27 | 江苏新河农用化工有限公司 | A kind of processing unit and method of the compound of class containing benzene dicarbonitrile tail gas |
| CN110845366B (en) * | 2019-12-03 | 2022-09-20 | 万华化学集团股份有限公司 | Preparation method and preparation system of chlorothalonil |
| CN111333032A (en) * | 2020-03-12 | 2020-06-26 | 江苏维尤纳特精细化工有限公司 | Environment-friendly recovery method of hydrogen chloride tail gas in chlorothalonil production |
| CN111282392A (en) * | 2020-03-23 | 2020-06-16 | 江苏新河农用化工有限公司 | Isophthalodinitrile dry-method trapping device and trapping method |
| CN111346469A (en) * | 2020-03-23 | 2020-06-30 | 江苏新河农用化工有限公司 | Isophthalonitrile wet-method trapping device and method |
-
2020
- 2020-07-17 CN CN202010694307.1A patent/CN111870988B/en active Active
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| CN111870988A (en) | 2020-11-03 |
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