CN206858468U - A kind of 3,4 2 chlorobenzotrifluoride continuous producing apparatus - Google Patents

A kind of 3,4 2 chlorobenzotrifluoride continuous producing apparatus Download PDF

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Publication number
CN206858468U
CN206858468U CN201720269705.2U CN201720269705U CN206858468U CN 206858468 U CN206858468 U CN 206858468U CN 201720269705 U CN201720269705 U CN 201720269705U CN 206858468 U CN206858468 U CN 206858468U
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China
Prior art keywords
liquid
chlorobenzotrifluoride
gas
bis
producing apparatus
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Withdrawn - After Issue
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CN201720269705.2U
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Chinese (zh)
Inventor
王德强
张鹏
于文智
赵贵敏
类成存
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SHANDONG DOCRIS CHEMICAL CO Ltd
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SHANDONG DOCRIS CHEMICAL CO Ltd
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Abstract

The utility model discloses one kind 3,4 two chlorobenzotrifluoride continuous producing apparatus, including entry mixers, the lower inlet of the outlet chlorination tower of the entry mixers, the top exit of the chlorination tower is communicated with gas-liquid separator, and the liquid-phase outlet of the gas-liquid separator is respectively communicated with the liquid phase feed import of product purification device and the entry mixers;Iron filler is filled with the chlorination tower.The utility model can effectively reduce catalyst change frequency compared with batch process and reduce the amount of dead catalyst iron cement, overcome the problem of batch process dead catalyst iron cement is difficult to handle, closure is realized in production, environmentally friendly;Continuous production can be not only realized, and portioned product circulation continues to react, and not only increases product yield, and raw material has been preheated, effectively using reaction heat, reduce energy consumption.

Description

A kind of chlorobenzotrifluoride continuous producing apparatus of 3,4- bis-
Technical field
It the utility model is related to technical field of chemical, and in particular to the chlorobenzotrifluoride continuous productions of 3,4- of one kind bis- are set It is standby.
Background technology
3,4 two chlorobenzotrifluorides are a kind of liquid of water white transparency, there is halogeno-benzene smell, not soluble in water, can be with benzene, first Benzene, ethanol, ether, halogenated hydrocarbons etc. are miscible.It is special that fluorine atom in the chlorobenzotrifluoride molecular structures of 3,4- bis- make it that it has Activity, it is important agricultural chemicals, medicine intermediate, can be used as the intermediate of insecticide ethiprole, it is fluorine-containing as synthesis diphenyl ether The intermediate of herbicide, it is widely used in the Minute Organic Synthesis such as medicine, agricultural chemicals, dyestuff field.
It is existing using p-chloro benzo trifluoride-99, chlorine as raw material, carry out chlorination reaction and produce the works of the chlorobenzotrifluorides of 3,4- bis- Skill, be a kind of batch process production equipment, reaction need could be carried out under the catalysis of iron ion, existing production method with iron powder, Ferric trichloride mixture is catalyst, produces the catalyst about 3kg that 1 ton of chlorobenzotrifluoride of 3,4- bis- needs, and solid catalyst is non- Fluid, conveying inconvenience, it is difficult to realize sealed feeding, catalyst charging process has volatile material spilling, to Workplace equipment Pipeline has corrosion, and employee's occupational health is harmful to, and reaction terminates also to need through sedimentation filtration separating catalyst, and that isolates urges Agent iron cement can not be reused, and reaction mass is also remained in iron cement, and storage and processing are difficult, be unfavorable for cleaning life Production, environmental pollution are serious.
Batch production process, a production cycle include the steps such as charging, reaction, discharging, auxiliary time of production length, reduced Utilization rate of equipment and installations, production capacity are low.Chlorination reaction is strong exothermal reaction, need to preheat raw material before batch process reaction, it is necessary to Thermal source is additionally provided, can not effectively utilize reaction heat, high energy consumption.
Chlorination reaction is especially carried out as raw material using p-chloro benzo trifluoride-99, chlorine and produces the chlorobenzotrifluorides of 3,4- bis-, target production The chlorobenzotrifluorides of thing 3,4- bis- are overchlorinated further to generate accessory substance 3,4,5-Trichloro-trifluoromethyl-benzene and 2,4,5- trichlorines three Toluene fluoride, speed and the target product 3 in chlorination reaction system of side reaction, the chlorobenzotrifluoride contents of 4- bis-, the amount of raw material chlorine, The factors such as reaction temperature, reaction time are relevant, and rate of side reactions is with the chlorobenzotrifluoride content liters of 3,4- in reaction system bis- High and accelerates, the quickening with reaction temperature rise is accelerated with the excess of raw material chlorine.Side reaction product increase can cause 3,4- Two chlorobenzotrifluoride yields decline, and accessory substance height also add the rectifying produce load of rear process, constrain the production of package unit Can, cause production cost high, economic benefit is low.If reduced by reducing in reaction system the chlorobenzotrifluoride contents of 3,4- bis- Accessory substance, unreacted raw material p-chloro benzo trifluoride-99 content can be caused high, increase rectifying load, restrict production capacity.
The content of the invention
Technical problem to be solved in the utility model is:In view of the deficienciess of the prior art, provide a kind of production effect Rate is high, utilization rate of equipment and installations is high, the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- that energy consumption is low, product yield is high.
In order to solve the above technical problems, the technical solution of the utility model is:
The chlorobenzotrifluoride continuous producing apparatus of 3,4- of one kind bis-, including entry mixers, the outlet of the entry mixers The lower inlet of chlorination tower is connected, the top exit of the chlorination tower is communicated with gas-liquid separator, the liquid of the gas-liquid separator Mutually outlet is respectively communicated with the liquid phase feed import of product purification device and the entry mixers;Iron is filled with the chlorination tower Matter filler.
As an improvement technical scheme, the gaseous phase outlet of the gas-liquid separator is communicated with tail chlorine tourie;It is described The inlet communication liquid charging stock storage tank of tail chlorine tourie;The liquid-phase outlet of the tail chlorine tourie connects the entry mixers Liquid phase feed import.
As further improved technical scheme, the gaseous phase outlet of the tail chlorine tourie is communicated with chlorination hydrogen retrieval dress Put.
As an improvement technical scheme, the liquid-phase outlet of the gas-liquid separator first passes through heat exchanger, then connects respectively The liquid phase feed import of logical product purification device and the entry mixers.
As an improvement technical scheme, be provided between the liquid phase feed import of the heat exchanger and the entry mixers Circulating pump.
As a kind of perferred technical scheme, the iron filler is filled out including iron plane flower filler, Pall ring filler, Raschig ring One or more of combinations in material, ladder ring packing, iron net body filler, iron ripple packing.
As an improvement technical scheme, the entry mixers are gas-liquid ejector.
As further improved technical scheme, the phase feed inlet communication of the gas-liquid ejector has gas buffer Tank.
As an improvement technical scheme, the chlorination tower includes multiple chlorination towers being serially connected;The charging is mixed The lower inlet for first chlorination tower that the outlet of clutch is serially connected, the top for the last chlorination tower being serially connected Outlet has gas-liquid separator.
As another improved technical scheme, the chlorination tower includes multiple circular response sections;Each circular response section Top be communicated with next section of circular response section bottom circulation line.
By adopting the above-described technical solution, the beneficial effects of the utility model are:
The chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- of the present utility model, including entry mixers, the charging mixing The lower inlet of the outlet chlorination tower of device, the top exit of the chlorination tower are communicated with gas-liquid separator, the gas-liquid point Liquid-phase outlet from device is respectively communicated with the liquid phase feed import of product purification device and the entry mixers;In the chlorination tower Filled with iron filler.Chlorination tower is entered back into after raw material is sufficiently mixed using entry mixers to react, and is improved continuous anti- Answer efficiency.Iron filler is filled with chlorination tower, filler can strengthen heat transfer and mass transfer of the material in tower, avoid temperature inequality from leading The problem of causing side reaction increase, catalyst of the iron filler as reaction is reusable, can effectively be reduced compared with batch process Catalyst change frequency and the amount for reducing dead catalyst iron cement, overcome the problem of batch process dead catalyst iron cement is difficult to handle, Closure is realized in production, is overcome batch process and is required to add iron powder, ferric chloride catalyst every time, opening charging has material steaming The problem of gas overflows, it is environmentally friendly.Continuous production can be not only realized, and portioned product recycling spraying emitter continues instead Should, product yield is not only increased, and raw material has been preheated, effectively using reaction heat, reduce energy consumption.
The gaseous phase outlet of the utility model gas-liquid separator is communicated with tail chlorine tourie;The import of the tail chlorine tourie connects Logical liquid charging stock storage tank;The liquid-phase outlet of the tail chlorine tourie connects the liquid phase feed import of the entry mixers, gas-liquid The waste gas utilization raw material p-chloro benzo trifluoride-99 that separator comes out absorbs to tail chlorine contained in tail gas, effectively improves chlorine Utilization rate, reduce the alkali lye dosage of vent gas treatment process, reduce the yield of sodium hypochlorite.
Entry mixers use gas-liquid ejector, the fierce mixing in gas-liquid ejector of raw material chlorine and p-chloro benzo trifluoride-99 Enter chlorination tower after uniformly, avoid local chlorine gas concentration height, local reaction fierceness temperature drift, solve continuous synthesis appearance The trichlorobenzotrifluoride of accessory substance 3,4,5- easily caused and 2,4,5- trichlorobenzotrifluoride contents rise, causes target product yield Reduce, after restriction the problem of process rectifying produce load.
Brief description of the drawings
The utility model is further illustrated with reference to the accompanying drawings and examples.
Fig. 1 is the structural representation of the utility model embodiment;
In figure, 1. entry mixers;2. chlorination tower;21. iron filler;3. gas-liquid separator;4. heat exchanger;5. tail chlorine is inhaled Closed cans;6. liquid charging stock storage tank;7. circulating pump;8. gas buffer tank;9. feed pump.
Embodiment
With reference to the accompanying drawings and examples, the utility model is expanded on further.It should be understood that these embodiments are merely to illustrate The utility model rather than limitation the scope of the utility model.In addition, it is to be understood that reading in the utility model instruction After appearance, those skilled in the art can make various changes or modifications to the utility model, and these equivalent form of values equally fall within this Apply for appended claims limited range.
As illustrated, the chlorobenzotrifluoride continuous producing apparatus of 3,4- of one kind bis-, including entry mixers 1, the charging are mixed The lower inlet of the outlet chlorination tower 2 of clutch 1, the top exit of the chlorination tower 2 is communicated with gas-liquid separator 3, described The liquid-phase outlet of gas-liquid separator 3 first passes through heat exchanger 4, then is respectively communicated with product purification device and the entry mixers 1 Liquid phase feed import;Iron filler 21 is filled with the chlorination tower 2.The gaseous phase outlet of the gas-liquid separator 3 is communicated with tail Chlorine tourie 5;The inlet communication liquid charging stock storage tank 6 of the tail chlorine tourie 5;The liquid-phase outlet of the tail chlorine tourie 5 connects Lead to the liquid phase feed import of the entry mixers 1.The gaseous phase outlet of the tail chlorine tourie 5 is communicated with chlorination hydrogen retrieval dress Put.Circulating pump 7 is provided between the liquid phase feed import of the heat exchanger 4 and the entry mixers 1.The entry mixers 1 Phase feed inlet communication has gas buffer tank 8.Set between the import of the liquid charging stock storage tank 6 and the tail chlorine tourie 5 There is feed pump 9.
As a preferred embodiment, the iron filler 21 includes iron plane flower filler, Pall ring filler, Raschig ring One or more of combinations in filler, ladder ring packing, iron net body filler, iron ripple packing.
As an improvement embodiment, the entry mixers 1 are gas-liquid ejector.
As an improvement embodiment, the chlorination tower 2 includes multiple chlorination towers being serially connected;The charging is mixed The lower inlet for first chlorination tower that the outlet of clutch is serially connected, the top for the last chlorination tower being serially connected Outlet has gas-liquid separator.
As another improved embodiment, the chlorination tower 2 includes multiple circular response sections;Each circular response section Top be communicated with next section of circular response section bottom circulation line.
Operation principle of the present utility model is:Chlorine from liquid chlorine vaporization enters gas buffer tank, through gas buffer tank Enter gas-liquid ejector after cushioning balance, raw material chlorine mixes with the liquid material that self-circulating pump is made in gas-liquid ejector Even, subsequently into chlorination tower, raw material fills in chlorination tower and chlorination reaction is carried out under the catalysis of iron filler, generates 3,4- dichloros Benzotrifluoride and hydrogen chloride, the mixtures of materials come out from chlorination tower enter gas-liquid separator, carry out gas-liquid separation, gas-liquid separation The material that device bottom comes out enters heat exchanger, and reaction heat is taken away by circulating hot water, goes out the material of heat exchanger, and a part is used as 3,4- Two chlorobenzotrifluoride crude products remove product purification device of refining, and a part enters gas-liquid injection as reaction cycle liquid by circulating pump Device, circular response is carried out, caused hydrogen chloride and a small amount of unreacted chlorine come out at the top of gas-liquid separator, subsequently into tail Chlorine tourie, unreacted a small amount of chlorine is absorbed with raw material p-chloro benzo trifluoride-99, from the hydrogen chloride of tail chlorine tourie top out Gas removes the chlorination hydrogen recovery unit of rear process, through three-level falling film absorption and alkali cleaning, absorbs the raw material of tail chlorine from tail chlorine tourie Bottom, which comes out, enters circulating pump, and the raw material in liquid charging stock storage tank is delivered to tail chlorine tourie through feed pump and absorbs tail chlorine.

Claims (10)

1. one kind 3, the chlorobenzotrifluoride continuous producing apparatus of 4- bis-, it is characterised in that:Including entry mixers, the charging mixing The lower inlet of the outlet chlorination tower of device, the top exit of the chlorination tower are communicated with gas-liquid separator, the gas-liquid point Liquid-phase outlet from device is respectively communicated with the liquid phase feed import of product purification device and the entry mixers;In the chlorination tower Filled with iron filler.
2. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 1, it is characterised in that:The gas-liquid separator Gaseous phase outlet be communicated with tail chlorine tourie;The inlet communication liquid charging stock storage tank of the tail chlorine tourie;The tail chlorine absorbs The liquid-phase outlet of tank connects the liquid phase feed import of the entry mixers.
3. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 2, it is characterised in that:The tail chlorine tourie Gaseous phase outlet be communicated with chlorination hydrogen recovery unit.
4. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 1, it is characterised in that:The gas-liquid separator Liquid-phase outlet first pass through heat exchanger, then be respectively communicated with the liquid phase feed import of product purification device and the entry mixers.
5. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 4, it is characterised in that:The heat exchanger and institute State and be provided with circulating pump between the liquid phase feed import of entry mixers.
6. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 1, it is characterised in that:The iron filler bag Include iron plane flower filler, Pall ring filler, Raschig ring filler, ladder ring packing, iron net body filler, one kind in iron ripple packing or Several combinations.
7. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as described in claim 1 to 6 any claim, its feature exist In:The entry mixers are gas-liquid ejector.
8. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 7, it is characterised in that:The gas-liquid ejector Phase feed inlet communication have gas buffer tank.
9. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 7, it is characterised in that:The chlorination tower includes Multiple chlorination towers being serially connected;The bottom for first chlorination tower that the outlet of the entry mixers is serially connected is entered Mouthful, the top exit for the last chlorination tower being serially connected is communicated with gas-liquid separator.
10. the chlorobenzotrifluoride continuous producing apparatus of 3,4- bis- as claimed in claim 7, it is characterised in that:The chlorination tower bag Include multiple circular response sections;The circulation pipe of the bottom of next section of circular response section is communicated with the top of each circular response section Road.
CN201720269705.2U 2017-03-18 2017-03-18 A kind of 3,4 2 chlorobenzotrifluoride continuous producing apparatus Withdrawn - After Issue CN206858468U (en)

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CN201720269705.2U CN206858468U (en) 2017-03-18 2017-03-18 A kind of 3,4 2 chlorobenzotrifluoride continuous producing apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201720269705.2U CN206858468U (en) 2017-03-18 2017-03-18 A kind of 3,4 2 chlorobenzotrifluoride continuous producing apparatus

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106892792A (en) * 2017-03-18 2017-06-27 山东道可化学有限公司 A kind of method for continuously synthesizing and its synthesis device of 3,4 2 chlorobenzotrifluoride
CN109970507A (en) * 2019-04-30 2019-07-05 山东道可化学有限公司 A kind of continuous production method and continuous producing apparatus of bis- chlorobenzotrifluoride of 3,4-

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106892792A (en) * 2017-03-18 2017-06-27 山东道可化学有限公司 A kind of method for continuously synthesizing and its synthesis device of 3,4 2 chlorobenzotrifluoride
CN106892792B (en) * 2017-03-18 2023-05-23 山东道可化学有限公司 Continuous synthesis method and equipment of 3, 4-dichloro benzotrifluoride
CN109970507A (en) * 2019-04-30 2019-07-05 山东道可化学有限公司 A kind of continuous production method and continuous producing apparatus of bis- chlorobenzotrifluoride of 3,4-
CN109970507B (en) * 2019-04-30 2022-09-27 山东道可化学有限公司 Continuous production method and continuous production equipment for 3, 4-dichlorobenzotrifluoride

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