CN109336062A - The device and method thereof of chlorine aether tail gas production chlorosulfuric acid - Google Patents

The device and method thereof of chlorine aether tail gas production chlorosulfuric acid Download PDF

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Publication number
CN109336062A
CN109336062A CN201811407118.0A CN201811407118A CN109336062A CN 109336062 A CN109336062 A CN 109336062A CN 201811407118 A CN201811407118 A CN 201811407118A CN 109336062 A CN109336062 A CN 109336062A
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China
Prior art keywords
chlorine
tail gas
gas
chlorosulfuric acid
condenser
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CN201811407118.0A
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Inventor
孙丰炜
谢圣斌
张良
刘嵩
王廷
孙丰春
毕义霞
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Shandong Kaisheng New Materials Co Ltd
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Shandong Kaisheng New Materials Co Ltd
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Priority to CN201811407118.0A priority Critical patent/CN109336062A/en
Publication of CN109336062A publication Critical patent/CN109336062A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/45Compounds containing sulfur and halogen, with or without oxygen
    • C01B17/4561Compounds containing sulfur, halogen and oxygen only
    • C01B17/4592Sulfuryl chloride (SO2Cl2)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/07Purification ; Separation
    • C01B7/0706Purification ; Separation of hydrogen chloride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Treating Waste Gases (AREA)

Abstract

The present invention relates to a kind of device and method thereof of chlorine aether tail gas production chlorosulfuric acid, belong to the field of tail gas treatment.The production method utilizes chlorine aether tail gas and excessive chlorine, carries out gas gas phase reaction.Chlorine ether device exhaust is successively by absorption tower, condenser, mist eliminator, into catalytic reactor, after catalysis reaction, by product condensed in two stages device, wherein liquid phase enters finished product storage tank, and gas phase portion squeezes into hydrochloric acid tank, unabsorbed gases recycled by water absorption processing.The device and method of chlorine aether tail gas production chlorosulfuric acid of the present invention not only reduce the discharge of exhaust gas, realize recycling for high-purity sulfur dioxide, and further improve the added value of product of hydrogen chloride in tail gas;Thus chlorosulfuric acid product purity >=98.5% prepared.

Description

The device and method thereof of chlorine aether tail gas production chlorosulfuric acid
Technical field
The invention belongs to tail gas disposal technique field, be specifically related to a kind of chlorine aether tail gas production chlorosulfuric acid equipment and its Method.
Background technique
Manufacturing enterprise carries out production chlorine ether using thionyl chloride method at present, and the tail gas that generation is reacted in production mainly contains chlorine Change hydrogen and sulfur dioxide, the country mainly carries out absorption processing to tail gas in a manner of water absorption, compression condensation, Alkali absorption.The party Method exists: (1) by-product impurity content is high, recycles difficult;(2) energy consumption is high, and it is long-term overstocked that output byproduct is difficult to sale; (3) larger to water and liquid alkaline consumption, it results in waste of resources.
Existing chlorosulfuric acid processing technique is often reacted with sterling sulfur dioxide and sterling chlorine, and chlorosulfuric acid, tool is made There is higher cost, the disadvantages of product purity is low.In chlorosulfuric acid production process, adds active carbon layer or camphor is catalyzed, it is right Production catalytic unit is more demanding, and structure is complicated and the storing dangerous degree of raw material is higher.
With production-scale continuous expansion, the reasonable processing method of a kind of pair of chlorine ether production tail gas is needed, tail gas is improved Absorb the value and reuse ratio of byproduct.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of equipment of chlorine aether tail gas production chlorosulfuric acid and side Method.This method not only reduces the discharge of exhaust gas, and gained chlorosulfuric acid product purity is higher, further improves dioxy in tail gas Change the added value of product of sulphur.
The equipment of chlorine aether tail gas production chlorosulfuric acid of the present invention, including chlorine aether tail gas pre-processing device, chlorosulfuric acid are raw Produce equipment and production tail gas treatment device;Chlorine aether tail gas pre-processing device includes absorption tower, tail gas condenser and mist eliminator;Sulfonyl Chlorine production equipment includes catalytic reactor, cycle condenser and chlorosulfuric acid finished product storage tank;Production tail gas treatment device includes that water is inhaled Receive treatment process and hydrochloric acid tank;Mist eliminator in chlorine aether tail gas pre-processing device passes through in pipeline and chlorosulfuric acid production equipment Catalytic reactor lower part side connects, and the second gas-liquid separator in chlorosulfuric acid production equipment passes through pipeline and production vent gas treatment Water in equipment absorbs treatment process connection, and water, which absorbs, passes through recycled pipeline and chlorine feed pipeline phase at the top for the treatment of process Even.
Wherein:
Chlorine aether tail gas pre-processing device further includes chlorine aether tail gas feeding line and absorbing liquid feeding line, absorbing liquid feed pipe Line is connect with absorption tower top side, and chlorine aether tail gas feeding line is connect with absorption tower lower part side, passes through pipe at the top of absorption tower Road is sequentially connected with tail gas condenser and mist eliminator.
Catalytic reactor lower part side is also connect with chlorine feed pipeline in chlorosulfuric acid production equipment, catalytic reactor lower part The other side is sequentially connected by pipeline and circulating pump and cycle condenser, and cycle condenser is upper by pipeline and catalytic reactor Portion's connection, catalytic reactor top are sequentially connected by pipeline and product first-stage condenser and the first gas-liquid separator, the first gas Liquid/gas separator liquid-phase outlet connect by pipeline with chlorosulfuric acid finished product storage tank, the first gas-liquid separator gaseous phase outlet pass through pipeline and Product secondary condenser and the second gas-liquid separator are sequentially connected, and the second gas-liquid separator liquid-phase outlet passes through pipeline and chlorosulfuric acid Finished product storage tank connection, the second gas-liquid separator gaseous phase outlet absorb treatment process with water by pipeline and connect.
The bottom that water absorbs treatment process in production tail gas treatment device is connect by pipeline with hydrochloric acid tank.
The specific effect of each equipment is as follows in the complete equipment of chlorine aether tail gas production chlorosulfuric acid of the present invention: absorbing Tower: the absorption to institute's chloroether in tail gas is completed by the spray of thionyl chloride and is dissolved.Tail gas condenser: it will be taken out of in absorption tower Partial oxidation sulfoxide carry out condensation liquefaction elimination.Mist eliminator: the thionyl chloride that tail gas condenser is taken out of is carried out to catch mist elimination. Catalytic reactor: catalysis reaction is carried out to excessive chlorine in the sulfur dioxide and chlorine gas transfer pipeline in tail gas, circulating pump is Reactor bottom hydrops, provides circulation power, squeezes into cycle condenser and is condensed.(product level-one is cold for two-step product condenser Condenser and product secondary condenser): it completes the liquefaction to discharge to top gaseous phase and condenses;Two-stage gas-liquid separator (the first gas-liquid point From device and the second gas-liquid separator) fixed gas is separated with product liquid after condensation.Chlorosulfuric acid finished product storage tank: to sulfonyl chlorine products into Row storage.Water absorbs treatment process: being absorbed with water to hydrogen chloride unreacted in tail gas, hydrochloric acid is made, squeeze into hydrochloric acid storage Tank, unreacted chlorine squeeze into recycled pipeline.
The method of chlorine aether tail gas production chlorosulfuric acid of the present invention, specifically includes the following steps:
One, chlorine aether tail gas pre-processes
(1) chlorine aether tail gas and absorbing liquid are in absorption tower after counter current contacting removal of impurities, and chlorine aether tail gas at the top of absorption tower by entering Tail gas condenser condensation, mist eliminator enter subsequent processing after catching mist;
Two, the preparation of chlorosulfuric acid
(2) from mist eliminator come out chlorine aether tail gas gas phase enter catalytic reactor, the sulfur dioxide in chlorine aether tail gas with into Enter the chlorine gas phase in catalytic reactor and carry out reaction to prepare chlorosulfuric acid, then by two-step product condenser and two-stage gas-liquid point After condensing and separating from device, the chlorosulfuric acid liquid phase of preparation squeezes into chlorosulfuric acid finished product storage tank, and gas phase enters production vent gas treatment process;
Three, the processing of tail gas is produced
(3) gas phase is after water absorbs treatment process processing, and liquid phase squeezes into hydrochloric acid tank, and gas phase enters recycled pipeline Recycled.
Wherein:
Based on mass fraction, chlorine aether tail gas consists of the following compositions: SO2: 62%, HCl:36%, chlorine ether: 2%.
The volume ratio of chlorine and chlorine aether tail gas is 3:5.Chlorine is excessive.
Absorbing liquid described in step (1) is thionyl chloride, tail gas condenser outlet temperature≤35 DEG C.
Catalytic reactor described in step (2) is connected with heating collet, controls catalytic reactor temperature at 50~80 DEG C, is catalyzed Reactor pressure≤19KPa controls gas phase residence time >=10s.
Two-step product condenser described in step (2) is product first-stage condenser and product secondary condenser, two-stage gas-liquid Separator is the first gas-liquid separator and the second gas-liquid separator, wherein product first-stage condenser outlet temperature≤55 DEG C, product Secondary condenser outlet temperature≤30 DEG C.
Chlorosulfuric acid finished product storage tank described in step (2) installs breather valve additional and is connected to a condenser, and controls condenser Outlet temperature≤25 DEG C.
Catalytic reactor bottom reaction solution described in step (2) squeezes into cycle condenser by circulating pump, cold through recycling Enter catalytic reactor top after condenser condensation to spray, cycle condenser outlet temperature≤45 DEG C.
Water described in step (3) absorbs treatment process for level Four absorption processing.
It is as follows that chlorine aether tail gas produces specific implementation process of the method for chlorosulfuric acid in production equipment:
(1) chlorine aether tail gas enters absorption tower by absorption tower lower part side, and thionyl chloride absorbing liquid is from absorption tower top side Into absorption tower, the two counter current contacting, thionyl chloride absorbing liquid absorbs the chlorine ether impurity in chlorine aether tail gas, then chlorine ether Tail gas is condensed by entering tail gas condenser at the top of absorption tower, and tail gas condenser outlet temperature is maintained at 35 DEG C hereinafter, by condensation Gas phase afterwards enters mist eliminator.
(2) enter catalytic reactor from the gas phase that mist eliminator comes out, entry site is tower body lower part side, excessive chlorine Gas phase is entered by chlorine feed pipeline from catalytic reactor lower part side, the sulfur dioxide in chlorine aether tail gas entered with lower part It is reacted, catalytic reactor bottom reaction solution squeezes into cycle condenser, cycle condenser outlet temperature≤45 by circulating pump DEG C, enter catalytic reactor top after cycle condenser condenses and spray, controls pressure≤19KPa, temperature in catalytic reactor At 50~80 DEG C, the chlorine aether tail gas residence time >=10s, chlorosulfuric acid is prepared.
(3) in the chlorosulfuric acid and chlorine aether tail gas prepared unreacted hydrogen chloride and excessive chlorine by the top of catalytic reactor Into product first-stage condenser condensation after enter the first gas-liquid separator separates, product first-stage condenser outlet temperature≤55 DEG C, The chlorosulfuric acid liquid phase condensed out enters chlorosulfuric acid finished product storage tank, the not condensed liquid phase got off and unreacted hydrogen chloride and chlorine Gas gas phase enters the progress gas-liquid separation of the second gas-liquid separator after entering the condensation of product secondary condenser, and product secondary condenser goes out Mouth temperature≤30 DEG C, liquid phase enter chlorosulfuric acid finished product storage tank, and gas phase enters water and absorbs treatment process.
(4) gas phase is after water absorbs treatment process processing, and the hydrochloric acid of preparation enters hydrochloric acid tank, and gas phase enters circulating sleeve With pipeline recycled, recycled pipeline is communicated with chlorine feed pipeline.
Compared with the prior art, the present invention has the following beneficial effects:
(1) device and method of chlorine aether tail gas production chlorosulfuric acid of the present invention not only reduce the discharge of exhaust gas, real Show recycling for high-purity sulfur dioxide, and further improves the added value of product of hydrogen chloride in tail gas;Thus Chlorosulfuric acid product purity >=98.5% of preparation.
(2) device of chlorine aether tail gas production chlorosulfuric acid of the present invention, it is structurally reasonable, it is highly-safe, it is easy to operate, if It is standby simple, small investment;The tail gas in the production of chlorine ether is cleverly utilized, not only can solve the qualified discharge problem of tail gas, but also can obtain To the higher sulfonyl chlorine products of purity, the economic two-win with environmental protection is realized.
Detailed description of the invention
Fig. 1 is the device figure of chlorine aether tail gas production chlorosulfuric acid of the present invention.
In figure: 1, chlorine aether tail gas feeding line;2, absorbing liquid feeding line;3, absorption tower;4, tail gas condenser;5, mist is caught Device;6, catalytic reactor;7, chlorine feed pipeline;8, circulating pump;9, cycle condenser;10, product first-stage condenser;11, One gas-liquid separator;12, product secondary condenser;13, the second gas-liquid separator;14, chlorosulfuric acid finished product storage tank;15, water absorbs Treatment process;16, hydrochloric acid tank;17, recycled pipeline.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
The equipment that chlorine aether tail gas described in the present embodiment 1 produces chlorosulfuric acid, including chlorine aether tail gas pre-processing device, chlorosulfuric acid Production equipment and production tail gas treatment device;Chlorine aether tail gas pre-processing device includes absorption tower 3, tail gas condenser 4 and mist eliminator 5;Chlorosulfuric acid production equipment includes catalytic reactor 6, cycle condenser 9 and chlorosulfuric acid finished product storage tank 14;Production vent gas treatment is set Standby includes that water absorbs treatment process 15 and hydrochloric acid tank 16;Mist eliminator 5 in chlorine aether tail gas pre-processing device passes through pipeline and sulphur 6 lower part side of catalytic reactor in acyl chlorides production equipment connects, and the second gas-liquid separator 13 in chlorosulfuric acid production equipment is logical It crosses pipeline and is connect with the water absorption treatment process 15 produced in tail gas treatment device, water, which absorbs, passes through circulation at the top for the treatment of process 15 Pipeline 17 is applied to be connected with chlorine feed pipeline 7.
Chlorine aether tail gas pre-processing device further includes chlorine aether tail gas feeding line 1 and absorbing liquid feeding line 2, absorbing liquid charging Pipeline 2 is connect with 3 top side of absorption tower, and chlorine aether tail gas feeding line 1 is connect with 3 lower part side of absorption tower, 3 top of absorption tower It is sequentially connected by pipeline and tail gas condenser 4 and mist eliminator 5.
6 lower part side of catalytic reactor is also connect with chlorine feed pipeline 7 in chlorosulfuric acid production equipment, catalytic reactor 6 The lower part other side is sequentially connected by pipeline with circulating pump 8 and cycle condenser 9, and cycle condenser 9 is anti-by pipeline and catalysis Answer the top of device 6 to connect, at the top of catalytic reactor 6 by pipeline and product first-stage condenser 10 and the first gas-liquid separator 11 according to Secondary connection, 11 liquid-phase outlet of the first gas-liquid separator are connect by pipeline with chlorosulfuric acid finished product storage tank 14, the first gas-liquid separator 11 gaseous phase outlets are sequentially connected by pipeline with product secondary condenser 12 and the second gas-liquid separator 13, the second gas-liquid separator 13 liquid-phase outlets are connect by pipeline with chlorosulfuric acid finished product storage tank 14, and 13 gaseous phase outlet of the second gas-liquid separator passes through pipeline and water Treatment process 15 is absorbed to connect.
The bottom that water absorbs treatment process 15 in production tail gas treatment device is connect by pipeline with hydrochloric acid tank 16.
Based on mass fraction, chlorine aether tail gas consists of the following compositions: SO2: 62%, HCl:36%, chlorine ether: 2%.
The volume ratio of chlorine and chlorine aether tail gas is 3:5.Chlorine is excessive.
The method that chlorine aether tail gas described in the present embodiment 1 produces chlorosulfuric acid, specifically includes the following steps:
(1) chlorine aether tail gas enters absorption tower 3 by 3 lower part side of absorption tower, and thionyl chloride absorbing liquid is from 3 top one of absorption tower Side enters absorption tower 3, the two counter current contacting, and thionyl chloride absorbing liquid absorbs the chlorine ether impurity in chlorine aether tail gas, then Chlorine aether tail gas is condensed by entering tail gas condenser 4 at the top of absorption tower 3, and 4 outlet temperature of tail gas condenser is maintained at 35 DEG C, through being subcooled Gas phase after solidifying enters mist eliminator 5.
(2) enter catalytic reactor 6 from the gas phase that mist eliminator 5 comes out, entry site is tower body lower part side, excessive chlorine Gas gas phase is entered by chlorine feed pipeline 7 from 6 lower part side of catalytic reactor, the dioxy in chlorine aether tail gas entered with lower part Change sulphur to be reacted, 6 bottom reaction solution of catalytic reactor squeezes into cycle condenser 9 by circulating pump 8, and cycle condenser 9 exports Temperature be 40 DEG C, through cycle condenser 9 condensation after enter 6 top of catalytic reactor spray, control catalytic reactor 6 in pressure≤ At 50 DEG C, the chlorine aether tail gas residence time is 15s, prepares chlorosulfuric acid for 19KPa, temperature.
(3) unreacted hydrogen chloride and excessive chlorine are pushed up by catalytic reactor 6 in the chlorosulfuric acid and chlorine aether tail gas prepared Portion, which enters after product first-stage condenser 10 condenses, enters the separation of the first gas-liquid separator 11,10 outlet temperature of product first-stage condenser It is 45 DEG C, the chlorosulfuric acid liquid phase condensed out enters chlorosulfuric acid finished product storage tank 14, the not condensed liquid phase got off and unreacted Hydrogen chloride and chlorine gas phase, which enter after product secondary condenser 12 condenses, enters the progress gas-liquid separation of the second gas-liquid separator 13, produces 12 outlet temperature of product secondary condenser is 30 DEG C, and liquid phase enters chlorosulfuric acid finished product storage tank 14, and gas phase enters water and absorbs treatment process 15。
(4) for gas phase after water absorbs the processing for the treatment of process 15, the hydrochloric acid of preparation enters hydrochloric acid tank 16, and gas phase, which enters, to be followed Ring set 17 recycled of pipeline, recycled pipeline 17 are communicated with chlorine feed pipeline 7.
Chlorosulfuric acid product purity prepared by embodiment 1 is 98.6%.
Embodiment 2
Based on mass fraction, chlorine aether tail gas consists of the following compositions: SO2: 62%, HCl:36%, chlorine ether: 2%.
The volume ratio of chlorine and chlorine aether tail gas is 3:5.Chlorine is excessive.
The method that chlorine aether tail gas described in the present embodiment 2 produces chlorosulfuric acid, specifically includes the following steps:
(1) chlorine aether tail gas enters absorption tower 3 by 3 lower part side of absorption tower, and thionyl chloride absorbing liquid is from 3 top one of absorption tower Side enters absorption tower 3, the two counter current contacting, and thionyl chloride absorbing liquid absorbs the chlorine ether impurity in chlorine aether tail gas, then Chlorine aether tail gas is condensed by entering tail gas condenser 4 at the top of absorption tower 3, and 4 outlet temperature of tail gas condenser is maintained at 32 DEG C, through being subcooled Gas phase after solidifying enters mist eliminator 5.
(2) enter catalytic reactor 6 from the gas phase that mist eliminator 5 comes out, entry site is tower body lower part side, excessive chlorine Gas gas phase is entered by chlorine feed pipeline 7 from 6 lower part side of catalytic reactor, the dioxy in chlorine aether tail gas entered with lower part Change sulphur to be reacted, 6 bottom reaction solution of catalytic reactor squeezes into cycle condenser 9 by circulating pump 8, and cycle condenser 9 exports Temperature be 43 DEG C, through cycle condenser 9 condensation after enter 6 top of catalytic reactor spray, control catalytic reactor 6 in pressure≤ At 65 DEG C, the chlorine aether tail gas residence time is 12s, prepares chlorosulfuric acid for 19KPa, temperature.
(3) unreacted hydrogen chloride and excessive chlorine are pushed up by catalytic reactor 6 in the chlorosulfuric acid and chlorine aether tail gas prepared Portion, which enters after product first-stage condenser 10 condenses, enters the separation of the first gas-liquid separator 11,10 outlet temperature of product first-stage condenser It is 50 DEG C, the chlorosulfuric acid liquid phase condensed out enters chlorosulfuric acid finished product storage tank 14, the not condensed liquid phase got off and unreacted Hydrogen chloride and chlorine gas phase, which enter after product secondary condenser 12 condenses, enters the progress gas-liquid separation of the second gas-liquid separator 13, produces 12 outlet temperature of product secondary condenser is 30 DEG C, and liquid phase enters chlorosulfuric acid finished product storage tank 14, and gas phase enters water and absorbs treatment process 15。
(4) for gas phase after water absorbs the processing for the treatment of process 15, the hydrochloric acid of preparation enters hydrochloric acid tank 16, and gas phase, which enters, to be followed Ring set 17 recycled of pipeline, recycled pipeline 17 are communicated with chlorine feed pipeline 7.
Chlorosulfuric acid product purity prepared by embodiment 2 is 98.5%.
Embodiment 3
Based on mass fraction, chlorine aether tail gas consists of the following compositions: SO2: 62%, HCl:36%, chlorine ether: 2%.
The volume ratio of chlorine and chlorine aether tail gas is 3:5.Chlorine is excessive.
The method that chlorine aether tail gas described in the present embodiment 3 produces chlorosulfuric acid, specifically includes the following steps:
(1) chlorine aether tail gas enters absorption tower 3 by 3 lower part side of absorption tower, and thionyl chloride absorbing liquid is from 3 top one of absorption tower Side enters absorption tower 3, the two counter current contacting, and thionyl chloride absorbing liquid absorbs the chlorine ether impurity in chlorine aether tail gas, then Chlorine aether tail gas is condensed by entering tail gas condenser 4 at the top of absorption tower 3, and 4 outlet temperature of tail gas condenser is maintained at 28 DEG C, through being subcooled Gas phase after solidifying enters mist eliminator 5.
(2) enter catalytic reactor 6 from the gas phase that mist eliminator 5 comes out, entry site is tower body lower part side, excessive chlorine Gas gas phase is entered by chlorine feed pipeline 7 from 6 lower part side of catalytic reactor, the dioxy in chlorine aether tail gas entered with lower part Change sulphur to be reacted, 6 bottom reaction solution of catalytic reactor squeezes into cycle condenser 9 by circulating pump 8, and cycle condenser 9 exports Temperature be 45 DEG C, through cycle condenser 9 condensation after enter 6 top of catalytic reactor spray, control catalytic reactor 6 in pressure≤ At 80 DEG C, the chlorine aether tail gas residence time is 10s, prepares chlorosulfuric acid for 19KPa, temperature.
(3) unreacted hydrogen chloride and excessive chlorine are pushed up by catalytic reactor 6 in the chlorosulfuric acid and chlorine aether tail gas prepared Portion, which enters after product first-stage condenser 10 condenses, enters the separation of the first gas-liquid separator 11,10 outlet temperature of product first-stage condenser It is 55 DEG C, the chlorosulfuric acid liquid phase condensed out enters chlorosulfuric acid finished product storage tank 14, the not condensed liquid phase got off and unreacted Hydrogen chloride and chlorine gas phase, which enter after product secondary condenser 12 condenses, enters the progress gas-liquid separation of the second gas-liquid separator 13, produces 12 outlet temperature of product secondary condenser is 30 DEG C, and liquid phase enters chlorosulfuric acid finished product storage tank 14, and gas phase enters water and absorbs treatment process 15。
(4) for gas phase after water absorbs the processing for the treatment of process 15, the hydrochloric acid of preparation enters hydrochloric acid tank 16, and gas phase, which enters, to be followed Ring set 17 recycled of pipeline, recycled pipeline 17 are communicated with chlorine feed pipeline 7.
Chlorosulfuric acid product purity prepared by embodiment 3 is 98.7%.

Claims (10)

1. a kind of equipment of chlorine aether tail gas production chlorosulfuric acid, it is characterised in that: raw including chlorine aether tail gas pre-processing device, chlorosulfuric acid Produce equipment and production tail gas treatment device;Chlorine aether tail gas pre-processing device includes absorption tower (3), tail gas condenser (4) and catches mist Device (5);Chlorosulfuric acid production equipment includes catalytic reactor (6), cycle condenser (9) and chlorosulfuric acid finished product storage tank (14);Production Tail gas treatment device includes that water absorbs treatment process (15) and hydrochloric acid tank (16);Mist eliminator in chlorine aether tail gas pre-processing device (5) it is connect with catalytic reactor (6) lower part side in chlorosulfuric acid production equipment by pipeline, the in chlorosulfuric acid production equipment Two gas-liquid separators (13) absorb treatment process (15) with the water produced in tail gas treatment device by pipeline and connect, at water absorption It is connected by recycled pipeline (17) with chlorine feed pipeline (7) at the top of science and engineering sequence (15).
2. the equipment of chlorine aether tail gas production chlorosulfuric acid according to claim 1, it is characterised in that: the pretreatment of chlorine aether tail gas is set Standby further includes chlorine aether tail gas feeding line (1) and absorbing liquid feeding line (2), absorbing liquid feeding line (2) on absorption tower (3) The connection of portion side, chlorine aether tail gas feeding line (1) connect with absorption tower (3) lower part side, pass through at the top of absorption tower (3) pipeline and Tail gas condenser (4) and mist eliminator (5) are sequentially connected.
3. the equipment of chlorine aether tail gas production chlorosulfuric acid according to claim 1, it is characterised in that: in chlorosulfuric acid production equipment Catalytic reactor (6) lower part side is also connect with chlorine feed pipeline (7), and catalytic reactor (6) lower part other side passes through pipeline It is sequentially connected with circulating pump (8) and cycle condenser (9), cycle condenser (9) passes through the top of pipeline and catalytic reactor (6) Connection, catalytic reactor (6) top are successively connected by pipeline with product first-stage condenser (10) and the first gas-liquid separator (11) It connects, the first gas-liquid separator (11) liquid-phase outlet is connect by pipeline with chlorosulfuric acid finished product storage tank (14), the first gas-liquid separator (11) gaseous phase outlet is sequentially connected by pipeline with product secondary condenser (12) and the second gas-liquid separator (13), the second gas-liquid Separator (13) liquid-phase outlet is connect by pipeline with chlorosulfuric acid finished product storage tank (14), the second gas-liquid separator (13) gaseous phase outlet Treatment process (15) are absorbed with water to connect.
4. the equipment of chlorine aether tail gas production chlorosulfuric acid according to claim 1, it is characterised in that: production tail gas treatment device The bottom that middle water absorbs treatment process (15) is connect by pipeline with hydrochloric acid tank (16).
5. a kind of method of chlorine aether tail gas production chlorosulfuric acid described in claim 1, it is characterised in that: specifically include following step It is rapid:
One, chlorine aether tail gas pre-processes
(1) chlorine aether tail gas and absorbing liquid be after absorption tower (3) interior counter current contacting removal of impurities, chlorine aether tail gas by the top of absorption tower (3) into Enter tail gas condenser (4) condensation, mist eliminator (5) enters subsequent processing after catching mist;
Two, the preparation of chlorosulfuric acid
(2) from mist eliminator (5) come out chlorine aether tail gas gas phase enter catalytic reactor (6), the sulfur dioxide in chlorine aether tail gas with Reaction is carried out into the chlorine gas phase in catalytic reactor (6) and prepares chlorosulfuric acid, then passes through two-step product condenser and two-stage After gas-liquid separator condenses and separates, the chlorosulfuric acid liquid phase of preparation squeezes into chlorosulfuric acid finished product storage tank (14), and gas phase enters production tail gas Treatment process;
Three, the processing of tail gas is produced
(3) gas phase is after water absorbs treatment process (15) processing, and liquid phase squeezes into hydrochloric acid tank (16), and gas phase enters recycled Pipeline (17) recycled.
6. the method for chlorine aether tail gas production chlorosulfuric acid according to claim 5, it is characterised in that: described in step (1) Absorbing liquid is thionyl chloride, tail gas condenser (4) outlet temperature≤35 DEG C;Catalytic reactor (6) described in step (2) is connected with liter Warm collet controls catalytic reactor (6) temperature at 50~80 DEG C, the interior pressure≤19KPa of catalytic reactor (6), and control gas phase is stopped Stay time >=10s.
7. the method for chlorine aether tail gas production chlorosulfuric acid according to claim 5, it is characterised in that: two described in step (2) Grade product condenser is product first-stage condenser (10) and product secondary condenser (12), and two-stage gas-liquid separator is the first gas-liquid Separator (11) and the second gas-liquid separator (13), wherein product first-stage condenser (10) outlet temperature≤55 DEG C, product second level Condenser (12) outlet temperature≤30 DEG C.
8. the method for chlorine aether tail gas production chlorosulfuric acid according to claim 5, it is characterised in that: described in step (2) Chlorosulfuric acid finished product storage tank (14) installs breather valve additional and is connected to a condenser, and controls condensator outlet temperature≤25 DEG C.
9. the method for chlorine aether tail gas production chlorosulfuric acid according to claim 5, it is characterised in that: described in step (2) Catalytic reactor (6) bottom reaction solution squeezes into cycle condenser (9) by circulating pump (8), condenses through cycle condenser (9) laggard Enter catalytic reactor (6) top spray, cycle condenser outlet temperature≤45 DEG C.
10. the method for chlorine aether tail gas production chlorosulfuric acid according to claim 5, it is characterised in that: described in step (3) Water absorbs treatment process (15) for level Four absorption processing.
CN201811407118.0A 2018-11-23 2018-11-23 The device and method thereof of chlorine aether tail gas production chlorosulfuric acid Withdrawn CN109336062A (en)

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CN201811407118.0A CN109336062A (en) 2018-11-23 2018-11-23 The device and method thereof of chlorine aether tail gas production chlorosulfuric acid

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Application Number Priority Date Filing Date Title
CN201811407118.0A CN109336062A (en) 2018-11-23 2018-11-23 The device and method thereof of chlorine aether tail gas production chlorosulfuric acid

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Application publication date: 20190215