CN206308011U - A kind of retracting device of hydrogen fluoride - Google Patents

A kind of retracting device of hydrogen fluoride Download PDF

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CN206308011U
CN206308011U CN201621398278.XU CN201621398278U CN206308011U CN 206308011 U CN206308011 U CN 206308011U CN 201621398278 U CN201621398278 U CN 201621398278U CN 206308011 U CN206308011 U CN 206308011U
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hydrogen fluoride
iii
low
gas
tourie
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李欣
温成元
都基清
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Inner Mongolia Ruimi Fine Chemical Co
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Inner Mongolia Ruimi Fine Chemical Co
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Abstract

The utility model discloses a kind of retracting device of hydrogen fluoride, belong to chemical production technical field.The retracting device includes low-pressure condenser, hydrogen fluoride recovery unit and gas absorbing unit;The low-pressure condenser is connected with reaction under high pressure system, the gas phase tail gas produced in reaction under high pressure system initially enters low-pressure condenser condensation, condensed liquid is reclaimed by low-pressure condenser outlet at bottom into hydrogen fluoride recovery unit, and not solidifying hydrogen chloride and hydrogen fluoride gas are by the top exit of low-pressure condenser into carrying out absorption treatment in gas absorbing unit;The hydrogen fluoride recovery unit includes being sequentially connected with low-pressure condenser outlet at bottom the hydrogen fluoride recycling can and hydrogen fluoride measuring tank for connecing.The device is kept apart using low-pressure condenser and by condenser during HF is reclaimed with reaction system, while equipment cost is reduced, it is thus also avoided that condenser occurs the phenomenon of leakage and coolant occurs and caused danger into reaction system.

Description

A kind of retracting device of hydrogen fluoride
Technical field
The utility model is related to chemical production technical field, and in particular to a kind of retracting device of hydrogen fluoride.
Background technology
Fluorine-containing pyridine organic compound is widely used in the production and living of people as important medicine, pesticide intermediate In.Fluorination reagent is used mostly two kinds of KF, anhydrous HF, and general fluorination reaction is that organic matter reacts with fluorination reagent, because KF is Inorganic salts, insoluble in organic solvent, are being needed to add solvent or catalyst using KF as fluorination reagent, and this is produced to organic fluoride The post processing of product increased many steps, and current most pyridines organic fluorination uses anhydrous HF as fluorination reagent.
Used as fluorination reagent, major part is high temperature, reaction under high pressure to anhydrous HF, produces high pressure to be accomplished by the excessive fluorination of input Hydrogen.Pyridinium chloride class compound is with anhydrous HF reaction generation HCl gases, it is necessary to row pressure during the course of the reaction, a large amount of by what is produced HCl gases discharge reaction system.
While hydrogen chloride is discharged, hydrogen fluoride is also discharged therewith, and this is accomplished by considering the recovery of hydrogen fluoride, at present fluorination What the recovery of hydrogen considered is to install high pressure condenser in the vapor delivery line of row pressure to reclaim HF, the HF of recovery enter reaction system after Continuous to participate in reaction, the problem for existing is that high pressure condenser needs cooling but medium cooling, leakage coolant occurs in high pressure condenser When, it may appear that coolant enters the phenomenon of reaction system, so as to cause danger.
Utility model content
For the above mentioned problem that existing chlorination class pyridine compounds in the art exist with anhydrous HF reaction fluorination hydrogen retrieval, this The purpose of utility model is to provide a kind of device for being fluorinated hydrogen retrieval, and the device is used for pyridinium chloride class compound and anhydrous HF The recovery of hydrogen fluoride in course of reaction, especially with excessive HF courses of reaction in, this reaction is mostly high-temperature high-voltage reaction.
The technical scheme that the utility model is used is as follows:
A kind of retracting device of hydrogen fluoride, including low-pressure condenser, hydrogen fluoride recovery unit and gas absorbing unit;It is described Low-pressure condenser is connected with reaction under high pressure system, and the gas phase tail gas produced in reaction under high pressure system initially enters low-pressure condenser Condensation, condensed liquid is reclaimed by low-pressure condenser outlet at bottom into hydrogen fluoride recovery unit, not solidifying hydrogen chloride With hydrogen fluoride gas by the top exit of low-pressure condenser into carrying out absorption treatment in gas absorbing unit;The hydrogen fluoride is returned Receiving unit includes being sequentially connected with low-pressure condenser outlet at bottom the hydrogen fluoride recycling can and hydrogen fluoride measuring tank for connecing.
The low-pressure condenser is connected with reaction under high pressure system by pipeline, and pressure-regulating valve, low pressure are set on pipeline The bottom of condenser is provided with air inlet, and the gas phase tail gas produced in reaction under high pressure system is via the pressure-regulating valve on pipeline from institute State air inlet to enter in low-pressure condenser, the chilled brine of -20 DEG C of low-pressure condenser confession.
The gas absorbing unit includes absorption tower I, tourie I, circulating pump I, absorption tower II, tourie II, circulating pump IIth, absorption tower III, tourie III, circulating pump III, alkali adsorption tower and alkali circulating pump;Wherein:Low-pressure condenser by main pipeline with Sulfuric acid drying unit is connected, be connected to respectively on main pipeline air inlet pipe I, air inlet pipe II, air inlet pipe III, air inlet pipe IV, branch road I, Branch road II and branch road III;Low-pressure condenser accesses the lower entrances on absorption tower I by air inlet pipe I, and absorption tower I connects absorption respectively Tank I and circulating pump I, tourie I are connected with circulating pump I;Washing, gas are circulated to material in absorption tower I by circulating pump I Body enters tourie I after water absorption, through washing nonabsorbable gas successively via branch road I, main pipeline and air inlet pipe II Into absorption tower II;
The absorption tower II connects tourie II and circulating pump II respectively, and tourie II is connected with circulating pump II;Pass through Circulating pump II is circulated washing to material in absorption tower II, and gas enters tourie II after water absorption, can not through washing The gas of absorption enters absorption tower III via branch road II, main pipeline and air inlet pipe III successively;
The absorption tower III connects tourie III and circulating pump III respectively, and tourie III is connected with circulating pump III;Pass through Circulating pump III is circulated washing to material in absorption tower III, and gas enters tourie III after water absorption, can not through washing The gas of absorption enters absorption alkali adsorption tower via branch road III, main pipeline and air inlet pipe IV successively;
Washing is circulated to material in alkali adsorption tower by alkali circulating pump, it is impossible to which the gas of absorption enters vent gas treatment dress Put.
80% liquid level running water is contained in the tourie I, tourie II and tourie III, total acid content is big in monitoring tank When 40%, it is transferred in the hydrochloric acid tank of tank field.
Gas is absorbed by the sodium hydroxide solution that concentration is 20% in the alkali adsorption tower.
The beneficial effects of the utility model are as follows:
The utility model device is isolated using low-pressure condenser and by condenser during HF is reclaimed with reaction system Open, while equipment cost is reduced, it is thus also avoided that condenser occurs the phenomenon of leakage and coolant occurs and sent out into reaction system It is raw dangerous.
Brief description of the drawings
Fig. 1 is that the utility model is fluorinated hydrogen recovery unit structural representation.
Fig. 2 is the gas absorbing unit structural representation in the utility model device.
In figure:1- reaction under high pressure systems;2- low-pressure condensers;3- gas absorbing units;4- hydrogen fluoride recycling cans;5- is fluorinated Hydrogen measuring tank;6- sulfuric acid drying units;300- main pipelines;301- air inlet pipe I;302- air inlet pipe II;303- air inlet pipe III;304- Air inlet pipe IV;311- absorption towers I;312- absorption towers II;313- absorption towers III;314- alkali adsorption towers;321- touries I;322- Tourie II;323- touries III;331- circulating pumps I;332- circulating pumps II;333- circulating pumps III;334- alkali circulating pumps;341- Branch road I;342- branch roads II;343- branch roads III.
Specific embodiment
Below in conjunction with detailed description the utility model.
The utility model is the device for being fluorinated hydrogen retrieval, it is adaptable to which organic matter prepares fluorine-containing pyridine with anhydrous hydrogen fluoride reaction The recovery of hydrogen fluoride during organic compound, its structure is as shown in Figure 1-2.The device is returned including low-pressure condenser 2, hydrogen fluoride Receive unit and gas absorbing unit 3;The low-pressure condenser 2 is connected with reaction under high pressure system 1, is produced in reaction under high pressure system 1 Raw gas phase tail gas initially enters low-pressure condenser 2 and condenses, and condensed liquid enters fluorination by the outlet at bottom of low-pressure condenser 2 Hydrogen retrieval unit is reclaimed, and solidifying hydrogen chloride and hydrogen fluoride gas are not inhaled by the top exit of low-pressure condenser 2 into gas Receiving in unit 3 carries out absorption treatment;The hydrogen fluoride recovery unit includes being sequentially connected what is connect with low-pressure condenser outlet at bottom Hydrogen fluoride recycling can 4 and hydrogen fluoride measuring tank 5.
The low-pressure condenser 2 is connected with reaction under high pressure system 1 by pipeline, and pressure-regulating valve is set on pipeline, low The bottom of condenser 2 is pressed to be provided with air inlet, the gas phase tail gas produced in reaction under high pressure system 1 is via the pressure-regulating valve on pipeline Enter in low-pressure condenser 2 from the air inlet, the chilled brine of -20 DEG C of low-pressure condenser confession.
The gas absorbing unit 3 includes absorption tower I 311, tourie I 321, circulating pump I 331, absorption tower II 312, suction The circulation of closed cans II 322, circulating pump II 332, absorption tower III 313, tourie III 323, circulating pump III 333, alkali adsorption tower 314 and alkali Pump 334;Wherein:Low-pressure condenser 2 is connected by main pipeline 300 with sulfuric acid drying unit 6, is connected to respectively on main pipeline 300 Air inlet pipe I 301, air inlet pipe II 302, air inlet pipe III 303, air inlet pipe IV 304, branch road I 341, branch road II 342 and branch road III 343; Low-pressure condenser 2 accesses the lower entrances on absorption tower I 311 by air inlet pipe I 301, and absorption tower I 311 connects tourie I respectively 321 and circulating pump I 331, tourie I 321 is connected with circulating pump I 331;By material in I 331 pairs of absorption towers I 311 of circulating pump Washing is circulated, gas enters tourie I 321 after water absorption, through washing nonabsorbable gas successively via branch road I 341st, main pipeline 300 and air inlet pipe II 302 enter absorption tower II 312;
The absorption tower II 312 connects tourie II 322 and circulating pump II 332, tourie II 322 and circulating pump II respectively 332 are connected;Washing is circulated by material in II 332 pairs of absorption towers II 312 of circulating pump, gas enters after water absorption Tourie II 322, enters via branch road II 342, main pipeline 300 and air inlet pipe III 303 successively through washing nonabsorbable gas Absorption tower III 313;
The absorption tower III 313 connects tourie III 323 and circulating pump III 333, tourie III 323 and circulating pump III respectively 333 are connected;Washing is circulated by material in III 333 pairs of absorption towers III 313 of circulating pump, gas enters after water absorption Tourie III 323, enters via branch road III 343, main pipeline 300 and air inlet pipe IV 304 successively through washing nonabsorbable gas Absorb alkali adsorption tower 314;
Washing is circulated to material in alkali adsorption tower 314 by alkali circulating pump 334, it is impossible to which the gas of absorption enters tail gas Processing unit.
80% liquid level running water is contained in the tourie I 321, tourie II 322 and tourie III 323, in monitoring tank When total acid content is more than 40%, it is transferred in the hydrochloric acid tank of tank field.
Embodiment 1
2- chloro-5-trifluoromethylpyridines with anhydrous hydrogen fluoride carry out that the chloro- 5- tri- of 2- are synthesized under the conditions of 170-190 DEG C Fluoromethylpyridin, is fluorinated excess hydrogen, and fluorination reaction produces gas phase tail gas to include 2- chloro-5-trifluoromethylpyridines, hydrogen chloride, fluorination Hydrogen etc..
Gas phase tail gas is condensed after being depressurized through pressure-reducing valve into low-pressure condenser, and the liquid under condensation enters fluorination hydrogen retrieval Tank, fixed gas hydrogen chloride and a small amount of hydrogen fluoride gas enter acid absorption column 1, by the circulating water wash of acid circulating pump 1, chlorine in gas phase Change hydrogen and a small amount of hydrogen fluoride gas enter sour tourie 1 after being only absorbed by the water, sour tourie is sampled once per hour, and monitoring total acid contains Amount, when total acid content is more than 40%, acid all goes to tank field storage tank, and unabsorbed hydrogen chloride and hydrogen fluoride enter acid and circulates Tower 2, enters back into sour recycle column 3, finally enters alkali recycle column 4;After the acid of sour tourie 1 is produced, the acid of sour tourie 2 is specially controlled Sour tourie 1, sour tourie 2 is gone to by the acid of sour tourie 3, and sour tourie 3 adds water to 80% liquid level;Hydrogen fluoride and hydrogen chloride Gas is all to be soluble in the gas for being dissolved in water, and the pollution in order to avoid tail gas to air finally sets alkali adsorption tower.
The amount that hydrogen fluoride is reclaimed per batch is the 1/3 of input amount.
The utility model is not limited to the present embodiment, any equivalent concepts in the technical scope that the utility model is disclosed Or change, it is classified as protection domain of the present utility model.

Claims (7)

1. a kind of retracting device of hydrogen fluoride, it is characterised in that:The retracting device includes low-pressure condenser, hydrogen fluoride recovery unit And gas absorbing unit;The low-pressure condenser is connected with reaction under high pressure system, the gas phase tail produced in reaction under high pressure system Gas initially enters low-pressure condenser condensation, and condensed liquid is entered by low-pressure condenser outlet at bottom into hydrogen fluoride recovery unit Row is reclaimed, and not solidifying hydrogen chloride and hydrogen fluoride gas are by the top exit of low-pressure condenser into being inhaled in gas absorbing unit Receipts treatment;The hydrogen fluoride recovery unit includes being sequentially connected with low-pressure condenser outlet at bottom the hydrogen fluoride recycling can and fluorine for connecing Change hydrogen measuring tank.
2. the retracting device of hydrogen fluoride according to claim 1, it is characterised in that:The low-pressure condenser and reaction under high pressure System is connected by pipeline, and pressure-regulating valve is set on pipeline, and the bottom of low-pressure condenser is provided with air inlet, reaction under high pressure system The gas phase tail gas produced in system enters in low-pressure condenser via the pressure-regulating valve on pipeline from the air inlet.
3. the retracting device of hydrogen fluoride according to claim 1, it is characterised in that:The gas absorbing unit includes absorbing Tower I, tourie I, circulating pump I, absorption tower II, tourie II, circulating pump II, absorption tower III, tourie III, circulating pump III, alkali Absorption tower and alkali circulating pump;Wherein:Low-pressure condenser is connected by main pipeline with sulfuric acid drying unit, is connect respectively on main pipeline There are air inlet pipe I, air inlet pipe II, air inlet pipe III, air inlet pipe IV, branch road I, branch road II and branch road III;Low-pressure condenser passes through air inlet Pipe I accesses the lower entrances on absorption tower I, and absorption tower I connects tourie I and circulating pump I respectively, and tourie I is connected with circulating pump I Connect;Washing is circulated to material in absorption tower I by circulating pump I, gas enters tourie I after water absorption, through washing Nonabsorbable gas enters absorption tower II via branch road I, main pipeline and air inlet pipe II successively.
4. the retracting device of hydrogen fluoride according to claim 3, it is characterised in that:The absorption tower II connects absorption respectively Tank II and circulating pump II, tourie II are connected with circulating pump II;Material in absorption tower II is circulated by circulating pump II Washing, gas enters tourie II after water absorption, through wash nonabsorbable gas successively via branch road II, main pipeline and Air inlet pipe III enters absorption tower III.
5. the retracting device of hydrogen fluoride according to claim 4, it is characterised in that:The absorption tower III connects absorption respectively Tank III and circulating pump III, tourie III are connected with circulating pump III;Material in absorption tower III is circulated by circulating pump III Washing, gas enters tourie III after water absorption, through wash nonabsorbable gas successively via branch road III, main pipeline and Air inlet pipe IV enters absorption alkali adsorption tower;Washing is circulated to material in alkali adsorption tower by alkali circulating pump, it is impossible to absorption Gas enters exhaust gas processing device.
6. the retracting device of hydrogen fluoride according to claim 3, it is characterised in that:The tourie I, tourie II and suction 80% liquid level running water is contained in closed cans III, when total acid content is more than 40% in monitoring tank, is transferred in the hydrochloric acid tank of tank field.
7. the retracting device of hydrogen fluoride according to claim 3, it is characterised in that:It is by concentration in the alkali adsorption tower 20% sodium hydroxide solution absorbs to gas.
CN201621398278.XU 2016-12-20 2016-12-20 A kind of retracting device of hydrogen fluoride Active CN206308011U (en)

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CN201621398278.XU CN206308011U (en) 2016-12-20 2016-12-20 A kind of retracting device of hydrogen fluoride

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Application Number Priority Date Filing Date Title
CN201621398278.XU CN206308011U (en) 2016-12-20 2016-12-20 A kind of retracting device of hydrogen fluoride

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112604418A (en) * 2020-12-12 2021-04-06 单县欣润化工有限公司 Method and system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112604418A (en) * 2020-12-12 2021-04-06 单县欣润化工有限公司 Method and system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas

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