CN118419857B - Device system and method for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation - Google Patents
Device system and method for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation Download PDFInfo
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- CN118419857B CN118419857B CN202410881712.2A CN202410881712A CN118419857B CN 118419857 B CN118419857 B CN 118419857B CN 202410881712 A CN202410881712 A CN 202410881712A CN 118419857 B CN118419857 B CN 118419857B
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- heat exchanger
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- hexachlorobenzene
- circulating heat
- hydrochloric acid
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 225
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 title claims abstract description 98
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 62
- 230000003647 oxidation Effects 0.000 title claims abstract description 47
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 47
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000010791 quenching Methods 0.000 claims abstract description 85
- 230000000171 quenching effect Effects 0.000 claims abstract description 85
- 238000005406 washing Methods 0.000 claims abstract description 54
- 239000012071 phase Substances 0.000 claims abstract description 31
- 238000004064 recycling Methods 0.000 claims abstract description 15
- 239000007791 liquid phase Substances 0.000 claims abstract description 10
- 239000012495 reaction gas Substances 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 23
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 19
- 239000000460 chlorine Substances 0.000 claims description 19
- 229910052801 chlorine Inorganic materials 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000003599 detergent Substances 0.000 claims description 16
- 238000007599 discharging Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 10
- 239000002736 nonionic surfactant Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 21
- 239000007787 solid Substances 0.000 abstract description 17
- 238000010828 elution Methods 0.000 abstract description 7
- 230000000903 blocking effect Effects 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 abstract 1
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 39
- 230000000052 comparative effect Effects 0.000 description 18
- 235000014113 dietary fatty acids Nutrition 0.000 description 16
- 229930195729 fatty acid Natural products 0.000 description 16
- 239000000194 fatty acid Substances 0.000 description 16
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 13
- 150000004665 fatty acids Chemical class 0.000 description 13
- 239000007789 gas Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 229930006000 Sucrose Natural products 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012948 isocyanate Substances 0.000 description 3
- 150000002513 isocyanates Chemical class 0.000 description 3
- 229950008882 polysorbate Drugs 0.000 description 3
- 229920000136 polysorbate Polymers 0.000 description 3
- 239000005720 sucrose Substances 0.000 description 3
- -1 sucrose fatty acid ester Chemical class 0.000 description 3
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229940117389 dichlorobenzene Drugs 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- RELMFMZEBKVZJC-UHFFFAOYSA-N 1,2,3-trichlorobenzene Chemical compound ClC1=CC=CC(Cl)=C1Cl RELMFMZEBKVZJC-UHFFFAOYSA-N 0.000 description 1
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical group ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- CELCMWUXMBTJRP-UHFFFAOYSA-N chlorobenzene;hydrochloride Chemical compound Cl.ClC1=CC=CC=C1 CELCMWUXMBTJRP-UHFFFAOYSA-N 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a device system and a method for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation, wherein the device system removes unreacted hydrogen chloride phase change heat and solution heat by arranging a circulating heat exchanger so as to concentrate hexachlorobenzene in a quenching device; the removal of hexachlorobenzene in the liquid phase is realized by arranging a filter and a washing system of a circulating heat exchanger; the filter and the circulating heat exchanger are switched on line to realize alternate operation, and then the washing system of the circulating heat exchanger is adopted to realize the elution and discharge of hexachlorobenzene, so that the blocking risk of the circulating heat exchanger is reduced, the stability of the device is improved, the solid content of byproduct hydrochloric acid can be reduced, and the problem of recycling the byproduct hydrochloric acid is solved.
Description
Technical Field
The invention relates to the technical field of reaction for preparing chlorine by hydrogen chloride oxidation, in particular to a device system and a method for removing hexachlorobenzene in the preparation of chlorine by hydrogen chloride oxidation.
Background
In the process for producing isocyanate by using the phosgene method, most chlorine atoms are discharged in the form of hydrogen chloride after carbonyl substitution reaction, and a large amount of byproduct hydrogen chloride brings great economic and environmental pressure to enterprises, so that the development of the isocyanate industry is directly restricted.
In order to solve the problem, the conventional methods for treating the byproduct hydrogen chloride comprise hydrochloric acid preparation by an absorption method, acid-base neutralization, production of products such as chloroethylene and the like, production of chlorine gas by hydrogen chloride oxidation by a Deacon method and the like. The Deacon method hydrogen chloride oxidation process is focused on realizing the recycling of chlorine resources, accords with the economic development mode of resource recycling, and is important for promoting the sustainable development of chlorine industry and protecting the environment. In addition, the Deacon method hydrogen chloride oxidation process has the advantages of no other side reactions, simple process flow, high efficiency and the like.
At present, the process of preparing chlorine by hydrogen chloride through oxidation of hydrogen chloride needs to adopt an upstream isocyanate byproduct hydrogen chloride, and the byproduct hydrogen chloride contains a large amount of chlorobenzene substances including monochlorobenzene, dichlorobenzene, trichlorobenzene and the like, so that the chlorobenzene substances need to be removed in order to obtain pure hydrogen chloride. CN 112121603a discloses a method and apparatus for removing chlorobenzene from hydrogen chloride gas, comprising removing chlorobenzene from hydrogen chloride gas containing chlorobenzene by gas membrane interception; the gas membrane is a composite membrane and comprises a casting bottom membrane and a selective layer membrane, has excellent performances of high flux and high retention rate, and can remarkably improve the chlorobenzene removal efficiency in HCl. Meanwhile, the modified activated carbon adsorbent loaded on the ZrO 2 sol is adopted to further reduce the chlorobenzene content in the HCl. CN 115006975A discloses a method for recycling hydrogen chloride in dichlorobenzene byproducts, which comprises the following steps: step one: washing by-product gas; step two: dechlorination of the byproduct gas; step three: absorbing and preparing acid; step four: separating organic phase; step five: removing benzene by resin adsorption; step six: desorbing and cooling; step seven: and (3) oxidizing and drying, and fully removing organic matters in the byproduct hydrochloric acid, so that relatively pure hydrogen chloride gas is obtained for a subsequent chlorosulfonic acid device. The method has the advantages that chlorobenzene or benzene is removed from raw material hydrogen chloride, the required process cost is high, various chlorobenzene is required to be intercepted, and the removal effect has certain limitation.
The byproduct hydrogen chloride is oxidized to generate hexachlorobenzene, so that the types of chlorobenzene are reduced, but the use of high-content chlorobenzene hydrogen chloride is still limited without removing the hexachlorobenzene in the reaction gas phase, and meanwhile, the byproduct hydrochloric acid has high solid content, so that the problems of serious blockage of a refining system of a device under high load, incapability of long-term operation and the like are caused.
Therefore, in view of the shortcomings of the prior art, it is highly desirable to provide a device system that can produce chlorine gas from high-content chlorobenzene-based hydrogen chloride as a raw material, effectively remove hexachlorobenzene, and ensure stability.
Disclosure of Invention
The invention aims to provide a device system and a method for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation, which can be used for removing hexachlorobenzene, reducing the blockage risk of a circulating heat exchanger, improving the stability of the device, reducing the solid content of byproduct hydrochloric acid to below 1ppm and solving the recycling problem of byproduct hydrochloric acid.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the invention provides a device system for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation, which comprises a condenser, a quenching device, a filter and a first pumping device which are sequentially connected along the flow direction of a material, wherein a liquid phase part discharged by the first pumping device is discharged, and part of the liquid phase part flows through a circulating heat exchanger and then returns to the quenching device;
The filter comprises a first filter and a second filter which are alternately operated; the circulating heat exchanger comprises a first circulating heat exchanger and a second circulating heat exchanger which alternately operate; the first circulating heat exchanger and the second circulating heat exchanger are respectively and independently connected with a detergent heater, and the detergent heater respectively and independently conveys detergent to the first circulating heat exchanger and the second circulating heat exchanger through a second pumping device; the second pumping device is connected with a waste liquid collector.
According to the device system for removing hexachlorobenzene in the chlorine gas prepared by hydrogen chloride oxidation, provided by the invention, unreacted hydrogen chloride phase change heat and solution heat are removed by arranging the circulating heat exchanger, so that the hexachlorobenzene is completely concentrated in the quenching device; the removal of hexachlorobenzene in the liquid phase is realized by arranging a filter and a washing system of a circulating heat exchanger; the on-line switching filter and the circulating heat exchanger are used for realizing the alternate operation, and then a washing system of the circulating heat exchanger is used for realizing the elution and discharge of hexachlorobenzene. The device system can remove hexachlorobenzene, reduce the blockage risk of the circulating heat exchanger and improve the stability of the device.
Preferably, the condenser is provided with a reaction gas phase inlet.
Preferably, the type of condenser comprises a tube heat exchanger or a plate heat exchanger;
The outlet of the condenser is connected with the bottom inlet of the quenching device;
The types of the quenching device comprise a packed tower, the number of the tower plates is 1-5, for example, 1,2, 3, 4 or 5, preferably 2-3;
The types of the circulating heat exchanger comprise shell-and-tube heat exchangers.
Preferably, the top of the quenching device is provided with a chlorine outlet.
Preferably, the type of filter includes any one of a basket filter, a bag filter or a cartridge filter, preferably a cartridge filter;
the filter may have a filtration accuracy of 0.5 to 40. Mu.m, for example, 0.5. Mu.m, 1. Mu.m, 3. Mu.m, 5. Mu.m, 10. Mu.m, 25. Mu.m, or 40. Mu.m, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable, preferably 1 to 5. Mu.m.
Preferably, the first pumping means comprises a first transfer pump.
Preferably, the second pumping means comprises a second transfer pump.
Preferably, the detergent heater is provided with a detergent inlet.
Preferably, the waste collector comprises a waste reservoir.
In a second aspect, the present invention provides a method for removing hexachlorobenzene from chlorine gas produced by hydrogen chloride oxidation, the method being performed by the apparatus system for removing hexachlorobenzene from chlorine gas produced by hydrogen chloride oxidation according to the first aspect, the method comprising the steps of:
Condensing and quenching the reaction gas phase obtained after the hydrogen chloride oxidation in sequence, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid back to the quenching after heat exchange;
Switching operation according to the pressure difference between the first filter and the second filter and washing the first filter and the second filter; and switching and operating the first circulating heat exchanger and the second circulating heat exchanger according to the bottom outlet temperature of the quenching device, and then circularly washing the circulating heat exchanger after heat exchange, and discharging the obtained washing liquid containing hexachlorobenzene.
According to the method for removing hexachlorobenzene in the chlorine gas prepared by hydrogen chloride oxidation, the cooling capacity of the circulating heat exchanger can be adjusted by monitoring the bottom outlet temperature of the quenching device; confirming the interception efficiency of hexachlorobenzene by monitoring the pressure difference between the first filter and the second filter and the bottom outlet temperature of the quenching device; the elution effect of hexachlorobenzene in the circulating heat exchanger is ensured by controlling the temperature and time of circulating washing. According to the method, the raw material hydrogen chloride with high content of chlorobenzene can be used, so that the diversity of raw material sources is ensured, and meanwhile, hexachlorobenzene can be removed, so that the blockage risk of a circulating heat exchanger is reduced, the removal efficiency of unreacted hydrogen chloride of a quenching system is improved, and the stability of the device is improved; the solid content of the byproduct hydrochloric acid can be reduced to be less than 1ppm, and the problem of recycling the byproduct hydrochloric acid is solved.
Preferably, the temperature of the condensed reaction gas phase is 80-180 ℃, for example, 80 ℃, 100 ℃, 130 ℃, 150 ℃ or 180 ℃, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable, preferably 100-150 ℃;
the outlet temperature of the bottom of the quenching device is 30-70 ℃, and the circulation volume of the bottom is 100-400t/h.
The bottom outlet temperature of the quenching apparatus may be 30-70 ℃, for example 30 ℃, 40 ℃, 50 ℃, 60 ℃ or 70 ℃, but is not limited to the values recited, and other values not recited in the range of values are equally applicable, preferably 30-50 ℃.
The bottom circulation of the quenching device is 100-400t/h, for example, 100t/h, 150t/h, 200t/h, 250t/h, 300t/h or 400t/h, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable, preferably 150-250t/h.
The amount of hydrochloric acid discharged from the part is 2-30t/h, for example, 2t/h, 5t/h, 10t/h, 20t/h, 25t/h or 30t/h, but not limited to the recited values, other non-recited values in the numerical range are equally applicable, preferably 5-20t/h, and the amount of hydrochloric acid recycled back to the quenching after heat exchange of the part is the bottom recycle amount of the quenching device.
Preferably, the chlorine obtained after the quenching is discharged from the top of the quenching device.
The temperature of the condensed reaction gas phase is controlled, so that hexachlorobenzene in the reaction gas phase is prevented from desublimation and is completely brought into a quenching device.
Preferably, the solute mass concentration of the hydrochloric acid is 15-32%, and the hexachlorobenzene content in the hydrochloric acid is 0.1-1ppm.
The solute mass concentration of the hydrochloric acid is 15-32%, for example, 15%, 20%, 25%, 30% or 32%, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The hexachlorobenzene content of the hydrochloric acid is 0.1 to 1ppm, and may be, for example, 0.1ppm, 0.3ppm, 0.5ppm, 0.8ppm or 1ppm, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, when the pressure difference between the first filter and the second filter is 50-250kPa, the first filter and the second filter are switched to operate;
when the bottom outlet temperature of the quenching device is 55-70 ℃, switching to operate the first circulating heat exchanger and the second circulating heat exchanger;
the outlet temperature of the circulating heat exchanger may be 20 to 60 ℃, for example 20 ℃, 30 ℃, 40 ℃,50 ℃ or 60 ℃, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable, preferably 20 to 40 ℃.
The pressure difference between the first filter and the second filter is 50 to 250kPa, for example, 50kPa, 100kPa, 150kPa, 200kPa or 250kPa, but not limited to the values recited, and other values not recited in the numerical range are equally applicable, and preferably 100 to 200kPa.
The bottom outlet temperature of the quenching apparatus may be 55-70 ℃, for example 55 ℃, 58 ℃, 60 ℃, 65 ℃ or 70 ℃, but is not limited to the values recited, and other values not recited in the range of values are equally applicable, preferably 55-60 ℃.
Preferably, the washing liquid used for the circulating washing comprises a nonionic surfactant aqueous solution with a solute mass concentration of 0.5-5%, for example, but not limited to, 0.5%, 1%, 1.5%, 2%, 3% or 5%, and other non-enumerated values within the numerical range are equally applicable, preferably 1-2%;
The solute in the nonionic surfactant aqueous solution comprises any one or a combination of at least two of sucrose fatty acid ester, fatty acid sorbitan or polysorbate, and typical but non-limiting combinations comprise a combination of sucrose fatty acid ester and fatty acid sorbitan, a combination of fatty acid sorbitan and polysorbate, or a combination of sucrose fatty acid ester, fatty acid sorbitan and polysorbate;
The washing liquid is obtained by heating at 60-100deg.C, and can be, for example, 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100deg.C, but not limited to the values listed, other non-listed values in the range are applicable, preferably 80-100deg.C;
The circulation quantity of the circulation washing is 100-250t/h, and the washing time is 10-60min.
The circulation amount of the circulating washing is 100-250t/h, for example, 100t/h, 150t/h, 180t/h, 200t/h or 250t/h, but is not limited to the recited values, and other non-recited values in the numerical range are equally applicable, preferably 150-200t/h.
The washing time of the cyclic washing is 10 to 60min, for example, 10min, 20min, 25min, 30min, 40min or 60min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable, preferably 20 to 30min.
Preferably, the draining is carried out when the turbidity content of the washing liquid containing hexachlorobenzene is more than 5%, and the washing liquid is additionally supplemented until the liquid level is constant.
The turbidity content of the hexachlorobenzene-containing washing liquor is > 5%, for example 6%, 8%, 9% or 10%, but is not limited to the values recited, other values not recited in the numerical range being equally applicable.
The term "turbidity" refers to the property of transparency or clarity of a solution, which refers to the scattering of light by suspended particles in the solution.
As a preferred technical solution of the method according to the invention, the method comprises the steps of:
sequentially condensing and quenching the reaction gas phase obtained after hydrogen chloride oxidation, discharging the obtained chlorine gas from the top of a quenching device, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid back to quenching after heat exchange;
the temperature of the condensed reaction gas phase is 80-180 ℃; the bottom outlet temperature of the quenching device is 30-70 ℃, and the bottom circulation amount is 100-400t/h; the solute mass concentration of the hydrochloric acid is 15-32%, and the hexachlorobenzene content in the hydrochloric acid is 0.1-1ppm;
When the pressure difference between the first filter and the second filter is 50-250kPa, switching operation and washing the first filter and the second filter; when the bottom outlet temperature of the quenching device is 55-70 ℃, switching to operate the first circulating heat exchanger and the second circulating heat exchanger; the outlet temperature of the circulating heat exchanger is 20-60 ℃; then, circularly washing the heat-exchanged circulating heat exchanger by adopting a nonionic surfactant aqueous solution with the solute mass concentration of 0.5-5% obtained after heating at the temperature of 60-100 ℃, wherein the circulation amount is 100-250t/h, and the washing time is 10-60min; discharging is carried out when the turbidity content of the obtained non-ionic surfactant aqueous solution containing hexachlorobenzene is more than 5%, and the non-ionic surfactant aqueous solution is additionally supplemented until the liquid level is constant.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the device system for removing hexachlorobenzene in the chlorine gas prepared by hydrogen chloride oxidation, provided by the invention, unreacted hydrogen chloride phase change heat and solution heat are removed by arranging the circulating heat exchanger, so that the hexachlorobenzene is completely concentrated in the quenching device; the removal of hexachlorobenzene in the liquid phase is realized by arranging a filter and a washing system of a circulating heat exchanger; the on-line switching filter and the circulating heat exchanger are used for realizing the alternate operation, and then a washing system of the circulating heat exchanger is used for realizing the elution and discharge of hexachlorobenzene;
(2) According to the method provided by the invention, the cooling capacity of the circulating heat exchanger can be adjusted by monitoring the bottom outlet temperature of the quenching device; confirming the interception efficiency of hexachlorobenzene by monitoring the pressure difference between the first filter and the second filter and the bottom outlet temperature of the quenching device; the elution effect of hexachlorobenzene in the circulating heat exchanger is ensured by controlling the temperature and time of circulating washing; according to the method, the raw material hydrogen chloride with high content of chlorobenzene can be used, so that the diversity of raw material sources is ensured, and meanwhile, hexachlorobenzene can be removed, so that the blockage risk of a circulating heat exchanger is reduced, the removal efficiency of unreacted hydrogen chloride of a quenching system is improved, and the stability of the device is improved; the solid content of the byproduct hydrochloric acid can be reduced to be less than 1ppm, and the problem of recycling the byproduct hydrochloric acid is solved.
Drawings
FIG. 1 is a schematic diagram of a system for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation according to example 1 of the present invention;
wherein: 1, a condenser; 2, a quenching device; 3, a first delivery pump; 4, a first filter; 5, a second filter; 6, a first circulating heat exchanger; 7, a second circulating heat exchanger; 8, a detergent heater; 9, a second delivery pump; 10, a waste liquid pond.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The chemicals in the examples below were all from the company enokak chemical, inc, analytically pure, commercially available.
The method for testing the content of chlorobenzene substances in hydrogen chloride comprises the following steps: the gas phase is adsorbed with chlorobenzene substances for a certain time by an adsorption tube, then is soaked and extracted by carbon disulfide, and the extracted oil phase is quantitatively analyzed by a 7890A gas chromatograph of Agilent company in America. Test conditions: adopting an ECD detector and an HP-5 chromatographic column, wherein the temperature of a sample inlet is 280 ℃, the flow rate of carrier gas (nitrogen) is 3mL/min, the split ratio is 50:1, the temperature of the detector is 280 ℃, and the flow rate of hydrogen is 30mL/min;
the method for testing the content of hexachlorobenzene in the discharged hydrochloric acid comprises the following steps: the hexachlorobenzene in the aqueous phase was extracted with n-hexane, and the upper oil phase was quantitatively analyzed by 7890A gas chromatograph from Agilent corporation of America. Test conditions: adopting an ECD detector and an HP-5 chromatographic column, wherein the temperature of a sample inlet is 280 ℃, the flow rate of carrier gas (nitrogen) is 3mL/min, the split ratio is 50:1, the temperature of the detector is 280 ℃, and the flow rate of hydrogen is 30mL/min;
The turbidity test method of the washing liquid comprises the following steps: the turbidity content in the washing liquid is measured by adopting a Hash TU5400SC online turbidity detector, so that the liquid to be tested is prevented from having bubbles or other impurities; the collected liquid sample is diluted by a certain multiple and placed in an optical pool of a turbidity detection instrument, the instrument emits light to pass through the sample, and the solution turbidity is obtained by taking the average value and multiplying the multiple by the three times of reading.
Example 1
The embodiment provides a device system for removing hexachlorobenzene in chlorine gas prepared by hydrogen chloride oxidation, as shown in fig. 1, the device system comprises a condenser 1, a quenching device 2, a filter and a first conveying pump 3 which are sequentially connected along the material flow direction, wherein a liquid phase part discharged by the first conveying pump 3 is discharged, and part of the liquid phase part flows through a circulating heat exchanger and then returns to the quenching device 2;
The filter comprises a first filter 4 and a second filter 5 which are alternately operated; the circulating heat exchangers comprise a first circulating heat exchanger 6 and a second circulating heat exchanger 7 which alternately operate; the first circulating heat exchanger 6 and the second circulating heat exchanger 7 are respectively and independently connected with a detergent heater 8, and the detergent heater 8 respectively and independently conveys detergent to the first circulating heat exchanger 6 and the second circulating heat exchanger 7 through a second conveying pump 9; the second delivery pump 9 is connected with a waste liquid pool 10;
The condenser 1 is a tubular heat exchanger; the type of the quenching device 2 is a packed tower with 3 trays; the type of the circulating heat exchanger is a shell-and-tube heat exchanger; the filter is a filter element filter with the filtering precision of 3 mu m; the condenser 1 is provided with a reaction gas phase inlet; the top of the quenching device 2 is provided with a chlorine outlet; the detergent heater 8 is provided with a detergent inlet.
Example 2
The present example provided a system for removing hexachlorobenzene in the production of chlorine by oxidation of hydrogen chloride, which was different from example 1 in that the type of the quenching apparatus 2 was a packed column having 1 tray number, the type of the filter was a basket filter having a filtration accuracy of 0.5. Mu.m, and the rest was the same as example 1.
Example 3
The present example provides a system for removing hexachlorobenzene in the production of chlorine by oxidation of hydrogen chloride, which is different from example 1 in that the type of the quenching apparatus 2 is a packed column having 5 trays, the type of the filter is a bag filter having a filtration accuracy of 40 μm, and the rest is the same as example 1.
Comparative example 1
This comparative example provides a system for removing hexachlorobenzene in the production of chlorine by oxidation of hydrogen chloride, which differs from example 1 in that the filter is adjusted to a continuously operating first filter 4, the circulation heat exchanger is adjusted to a continuously operating first circulation heat exchanger 6, the first circulation heat exchanger 6 is not connected with a detergent heater 8 and a second transfer pump 9, and the rest is the same as example 1.
Comparative example 2
This comparative example provides a system for removing hexachlorobenzene in the production of chlorine by oxidation of hydrogen chloride, which differs from example 1 in that the circulating heat exchanger is adjusted to a continuously operated first circulating heat exchanger 6, the first circulating heat exchanger 6 is not connected to a detergent heater 8 and a second transfer pump 9, and the rest is the same as example 1.
Comparative example 3
This comparative example provides a system for removing hexachlorobenzene in the production of chlorine by oxidation of hydrogen chloride, which differs from example 1 in that it is identical to example 1 except that the filter is adjusted to the first filter 4 which is operated continuously.
Application example 1
The application example provides a method for removing hexachlorobenzene from chlorine gas prepared by hydrogen chloride oxidation by using the device system provided in the embodiment 1, wherein the method comprises the following steps:
Condensing the reaction gas phase obtained after the oxidation of the hydrogen chloride with the chlorobenzene content of 15ppm to obtain a reaction gas phase at 100 ℃, quenching the reaction gas phase, discharging the obtained chlorine from the top of a quenching device 2, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid back to the quenching after heat exchange; the bottom circulation amount of the quenching device 2 is 200t/h, and the hydrochloric acid amount of partial discharged hydrochloric acid is 10t/h; the solute mass concentration of the hydrochloric acid is 20%;
In the quenching process, when the pressure difference between the first filter 4 and the second filter 5 is 200kPa, the operation filter is switched and the washing replacement is carried out; when the bottom outlet temperature of the quenching device 2 is 58 ℃, switching to operate a circulating heat exchanger, wherein the outlet temperature of the circulating heat exchanger is 30 ℃; then, the circulating heat exchanger after heat exchange is circularly washed by adopting the fatty acid sorbitan aqueous solution with the solute mass concentration of 2 percent, which is obtained after heating at 90 ℃, wherein the circulating amount is 200t/h, and the washing time is 25min; the discharge is carried out when the turbidity content of the obtained hexachlorobenzene-containing fatty acid sorbitan aqueous solution is 6%, and the fatty acid sorbitan aqueous solution is additionally supplemented until the liquid level is constant.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.1ppm, the device system can realize long-time high-load stable operation, and the problem of blockage of the circulating heat exchanger is solved.
Application example 2
The application example provides a method for removing hexachlorobenzene from chlorine gas prepared by hydrogen chloride oxidation by using the device system provided in the embodiment 1, wherein the method comprises the following steps:
Condensing the reaction gas phase obtained after the oxidation of the hydrogen chloride with the chlorobenzene content of 10ppm to obtain a reaction gas phase at 80 ℃, quenching the reaction gas phase, discharging the obtained chlorine from the top of a quenching device 2, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid back to the quenching after heat exchange; the bottom circulation volume of the quenching device 2 is 100t/h, and the volume of hydrochloric acid discharged from part of the quenching device is 30t/h; the solute mass concentration of the hydrochloric acid is 32%;
In the quenching process, when the pressure difference between the first filter 4 and the second filter 5 is 50kPa, the operation filter is switched and the washing replacement is carried out; when the bottom outlet temperature of the quenching device 2 is 55 ℃, switching to operate a circulating heat exchanger, wherein the outlet temperature of the circulating heat exchanger is 20 ℃; then, the circulating heat exchanger after heat exchange is circularly washed by adopting the fatty acid sorbitan aqueous solution with the solute mass concentration of 5 percent, which is obtained after heating at 60 ℃, the circulating amount is 250t/h, and the washing time is 10min; the discharge is carried out when the turbidity content of the obtained hexachlorobenzene-containing fatty acid sorbitan aqueous solution is 8%, and the fatty acid sorbitan aqueous solution is additionally supplemented until the liquid level is constant.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.3ppm, the device system can realize long-time high-load stable operation, and the problem of blockage of the circulating heat exchanger is solved.
Application example 3
The application example provides a method for removing hexachlorobenzene from chlorine gas prepared by hydrogen chloride oxidation by using the device system provided in the embodiment 1, wherein the method comprises the following steps:
condensing the reaction gas phase obtained after the oxidation of the hydrogen chloride with the chlorobenzene content of 20ppm to obtain a reaction gas phase at 180 ℃, then quenching, discharging the obtained chlorine from the top of a quenching device 2, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid to the quenching after heat exchange; the bottom circulation amount of the quenching device 2 is 400t/h, and the hydrochloric acid amount of partial discharged hydrochloric acid is 2t/h; the solute mass concentration of the hydrochloric acid is 15%;
In the quenching process, when the pressure difference between the first filter 4 and the second filter 5 is 250kPa, the operation filter is switched and the washing replacement is carried out; when the bottom outlet temperature of the quenching device 2 is 70 ℃, switching to operate a circulating heat exchanger, wherein the outlet temperature of the circulating heat exchanger is 60 ℃; then, the circulating heat exchanger after heat exchange is circularly washed by adopting the fatty acid sorbitan aqueous solution with the solute mass concentration of 0.5 percent obtained after heating at 100 ℃, the circulating amount is 100t/h, and the washing time is 60min; the discharge is carried out when the turbidity content of the obtained hexachlorobenzene-containing fatty acid sorbitan aqueous solution is 9%, and the fatty acid sorbitan aqueous solution is additionally supplemented until the liquid level is constant.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.5ppm, the device system can realize long-time high-load stable operation, and the problem of blockage of the circulating heat exchanger is solved.
Application example 4
The application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation by using the device system provided in application example 1, which is different from application example 1 in that the temperature of the condensed reaction gas phase is controlled to be 60 ℃, and the rest is the same as application example 1.
In the application example, the solid content of hexachlorobenzene in the externally discharged hydrochloric acid is 0.1ppm, and the temperature of the reaction gas phase after condensation is controlled to be too low, so that the outlet of a condenser is blocked, the heat exchange efficiency is continuously reduced, and the final device system cannot operate under high load, and gradually reduces the load until the device system is stopped.
Application example 5
The application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation by using the device system provided in application example 1, which is different from application example 1 in that the temperature of the condensed reaction gas phase is controlled to be 190 ℃, and the rest is the same as application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.8ppm, and the temperature of the reaction gas phase after condensation is controlled to be too high, so that the hexachlorobenzene cannot be completely condensed in a quenching system, and the top demister is blocked and brought from the top to the downstream to influence the product quality.
Application example 6
The present application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation using the apparatus system provided in application example 1, which is different from application example 1 in that when the pressure difference between the first filter 4 and the second filter 5 is 40kPa, the operation filter is switched and the replacement is washed, and the rest is the same as application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.1ppm, and the frequent switching of the filters can be caused by the fact that the pressure difference between the first filter and the second filter is controlled to be too small, so that the running cost is increased.
Application example 7
The present application example provided a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation using the apparatus system provided in application example 1, which was different from application example 1 in that when the pressure difference between the first filter 4 and the second filter 5 was 260kPa, the operation filter was switched and the replacement was washed, and the rest was the same as in application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 1.2ppm, and the filtration effect is reduced and the content of hexachlorobenzene in the byproduct hydrochloric acid is increased due to the fact that the pressure difference between the first filter and the second filter is controlled to be too large.
Application example 8
The application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation by using the device system provided in application example 1, which is different from application example 1 in that when the bottom outlet temperature of the quenching device 2 is 45 ℃, the operation of the circulating heat exchanger is switched, and the rest is the same as application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.1ppm, and the circulating heat exchanger is switched and cleaned frequently due to the fact that the circulating heat exchanger is switched and operated when the bottom outlet temperature of the quenching device is too low, so that the operation cost is increased.
Application example 9
The application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation by using the device system provided in application example 1, which is different from application example 1 in that when the bottom outlet temperature of the quenching device 2 is 80 ℃, the operation of the circulating heat exchanger is switched, and the rest is the same as application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.3ppm, and the bottom outlet temperature of the quenching device is too high to switch and operate the circulating heat exchanger, so that the bottom temperature of the quenching device gradually rises, the device system cannot operate under high load, and the load is gradually reduced until the quenching device is stopped.
Application example 10
The application example provides a method for removing hexachlorobenzene from chlorine gas prepared by hydrogen chloride oxidation by using the device system provided in the application example 2, and the steps of the method are the same as those of the application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 0.1ppm, the accuracy of a filter element of the filter is higher, the pressure difference of the filter is increased fast, the switching is frequent, the running cost is increased, the device system can realize long-time high-load stable running, and the problem of blockage of a circulating heat exchanger is solved.
Application example 11
The application example provides a method for removing hexachlorobenzene from chlorine gas prepared by hydrogen chloride oxidation by using the device system provided in the application example 3, and the steps of the method are the same as those of application example 1.
In the application example, the solid content of hexachlorobenzene in the discharged hydrochloric acid is 1.1ppm, the precision of a filter element of a filter is low, the switching and cleaning frequency of the circulating heat exchanger is high, the running cost is increased, the device system can realize long-time high-load stable running, and the blockage problem of the circulating heat exchanger is solved.
Comparative application example 1
The comparative application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation using the apparatus system provided in comparative example 1, which is different from application example 1 in that there is no step of switching operation of the filter and washing replacement, there is no step of switching operation of the circulation heat exchanger and circulation washing, and the rest is the same as application example 1.
In the comparative application example, the filter/circulating heat exchanger is blocked, the content of hexachlorobenzene in hydrochloric acid is continuously increased, the discharge is limited, the temperature at the bottom of the quenching device is continuously increased, the device system cannot operate under high load, the load is gradually reduced until the device is stopped, the content of hexachlorobenzene in the discharged hydrochloric acid reaches 500ppm, and the hydrochloric acid cannot be recycled.
Comparative application example 2
The comparative application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation using the apparatus system provided in comparative example 2, which is different from application example 1 in that there is no step of switching operation of the circulation heat exchanger and circulation washing, and the rest is the same as application example 1.
In the comparative application example, the hexachlorobenzene content in the externally discharged hydrochloric acid is not detected, but the heat exchange efficiency of the circulating heat exchanger is gradually reduced, the bottom temperature of the quenching device is gradually increased, the device system cannot operate under high load, and the load is gradually reduced until the vehicle stops.
Comparative application example 3
The comparative application example provides a method for removing hexachlorobenzene from chlorine gas by hydrogen chloride oxidation using the apparatus system provided in comparative example 3, which is different from application example 1 in that there is no step of switching operation filter and washing replacement, and the rest is the same as application example 1.
In the comparative application example, the filter is blocked, the discharged hydrochloric acid is limited, the content of hexachlorobenzene in the discharged hydrochloric acid reaches 20ppm, the hydrochloric acid can not be recycled, the device system can not run under high load, and the load is gradually reduced until the device system is stopped.
In summary, according to the device system for removing hexachlorobenzene in preparing chlorine by oxidizing hydrogen chloride, provided by the invention, the circulating heat exchanger is arranged to remove unreacted hydrogen chloride phase-change heat and solution heat, so that hexachlorobenzene is completely concentrated in the quenching device; the removal of hexachlorobenzene in the liquid phase is realized by arranging a filter and a washing system of a circulating heat exchanger; the on-line switching filter and the circulating heat exchanger are used for realizing the alternate operation, and then a washing system of the circulating heat exchanger is used for realizing the elution and discharge of hexachlorobenzene;
According to the method provided by the invention, the cooling capacity of the circulating heat exchanger can be adjusted by monitoring the bottom outlet temperature of the quenching device; confirming the interception efficiency of hexachlorobenzene by monitoring the pressure difference between the first filter and the second filter and the bottom outlet temperature of the quenching device; the elution effect of hexachlorobenzene in the circulating heat exchanger is ensured by controlling the temperature and time of circulating washing; according to the method, the raw material hydrogen chloride with high content of chlorobenzene can be used, so that the diversity of raw material sources is ensured, and meanwhile, hexachlorobenzene can be removed, so that the blockage risk of a circulating heat exchanger is reduced, the removal efficiency of unreacted hydrogen chloride of a quenching system is improved, and the stability of the device is improved; the solid content of the byproduct hydrochloric acid can be reduced to be less than 1ppm, and the problem of recycling the byproduct hydrochloric acid is solved.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present invention disclosed herein are within the scope of the present invention.
Claims (10)
1. The device system for removing hexachlorobenzene in preparing chlorine by hydrogen chloride oxidation is characterized by comprising a condenser, a quenching device, a filter and a first pumping device which are sequentially connected along the material flow direction, wherein a liquid phase part discharged by the first pumping device is discharged outwards, and a part of the liquid phase part flows through a circulating heat exchanger and then returns to the quenching device;
discharging chlorine from the top of the quenching device, and obtaining hydrochloric acid containing solid-phase hexachlorobenzene from the bottom of the quenching device;
The filter comprises a first filter and a second filter which are alternately operated; the circulating heat exchanger comprises a first circulating heat exchanger and a second circulating heat exchanger which alternately operate; the first circulating heat exchanger and the second circulating heat exchanger are respectively and independently connected with a detergent heater, and the detergent heater respectively and independently conveys detergent to the first circulating heat exchanger and the second circulating heat exchanger through a second pumping device; the second pumping device is connected with a waste liquid collector.
2. The plant arrangement according to claim 1, characterized in that the kind of condenser comprises a tube heat exchanger or a plate heat exchanger;
The quenching device comprises a packed tower, wherein the number of tower plates is 1-5;
The types of the circulating heat exchanger comprise shell-and-tube heat exchangers.
3. The device system of claim 1, wherein the type of filter comprises any one of a basket filter, a bag filter, or a cartridge filter;
the filter has a filtration accuracy of 0.5-40 μm.
4. A method for removing hexachlorobenzene from chlorine gas produced by hydrogen chloride oxidation, characterized in that the method is carried out by the apparatus system for removing hexachlorobenzene from chlorine gas produced by hydrogen chloride oxidation according to any one of claims 1 to 3, comprising the steps of:
Condensing and quenching the reaction gas phase obtained after the hydrogen chloride oxidation in sequence, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid back to the quenching after heat exchange;
Switching operation according to the pressure difference between the first filter and the second filter and washing the first filter and the second filter; and switching and operating the first circulating heat exchanger and the second circulating heat exchanger according to the bottom outlet temperature of the quenching device, and then circularly washing the circulating heat exchanger after heat exchange, and discharging the obtained washing liquid containing hexachlorobenzene.
5. The process of claim 4, wherein the temperature of the condensed reaction gas phase is from 80 ℃ to 180 ℃;
the outlet temperature of the bottom of the quenching device is 30-70 ℃, and the circulation volume of the bottom is 100-400t/h.
6. The method according to claim 4, wherein the solute mass concentration of the hydrochloric acid is 15-32%, and the hexachlorobenzene content in the hydrochloric acid is 0.1-1ppm.
7. The method of claim 4, wherein the first filter and the second filter are switched to operate when the pressure difference between the first filter and the second filter is 50kPa to 250 kPa;
when the bottom outlet temperature of the quenching device is 55-70 ℃, switching to operate the first circulating heat exchanger and the second circulating heat exchanger;
the outlet temperature of the circulating heat exchanger is 20-60 ℃.
8. The method according to claim 4, wherein the washing liquid used for the circulating washing comprises a nonionic surfactant aqueous solution having a solute mass concentration of 0.5 to 5%;
The washing liquid is obtained after heating at 60-100 ℃;
The circulation quantity of the circulation washing is 100-250t/h, and the washing time is 10-60min.
9. The process according to claim 4, wherein the discharge is carried out at a turbidity content of > 5% of the hexachlorobenzene-containing washing liquor, while additionally replenishing the washing liquor to a constant liquid level.
10. The method according to claim 4, characterized in that it comprises the steps of:
Condensing and quenching the reaction gas phase obtained after the hydrogen chloride oxidation in sequence, filtering the obtained hydrochloric acid, discharging part of the hydrochloric acid, and recycling part of the hydrochloric acid back to the quenching after heat exchange;
the temperature of the condensed reaction gas phase is 80-180 ℃; the bottom outlet temperature of the quenching device is 30-70 ℃, and the bottom circulation amount is 100-400t/h; the solute mass concentration of the hydrochloric acid is 15-32%, and the hexachlorobenzene content in the hydrochloric acid is 0.1-1ppm;
When the pressure difference between the first filter and the second filter is 50-250kPa, switching operation and washing the first filter and the second filter; when the bottom outlet temperature of the quenching device is 55-70 ℃, switching to operate the first circulating heat exchanger and the second circulating heat exchanger; the outlet temperature of the circulating heat exchanger is 20-60 ℃; then, circularly washing the heat-exchanged circulating heat exchanger by adopting a nonionic surfactant aqueous solution with the solute mass concentration of 0.5-5% obtained after heating at the temperature of 60-100 ℃, wherein the circulation amount is 100-250t/h, and the washing time is 10-60min; discharging is carried out when the turbidity content of the obtained non-ionic surfactant aqueous solution containing hexachlorobenzene is more than 5%, and the non-ionic surfactant aqueous solution is additionally supplemented until the liquid level is constant.
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| CN112121603A (en) * | 2019-06-24 | 2020-12-25 | 万华化学集团股份有限公司 | Method and device for removing chlorobenzene from hydrogen chloride gas |
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| CN109911862B (en) * | 2019-03-18 | 2021-05-07 | 昆明理工大学 | Gas-solid separation method and system for elemental sulfur in sulfur-containing tail gas |
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| CN117398812B (en) * | 2023-12-15 | 2024-02-13 | 万华化学集团股份有限公司 | Quenching absorption method for aromatic hydrocarbon ammoxidation reaction gas |
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| CN107827080A (en) * | 2017-11-16 | 2018-03-23 | 新疆中泰新鑫化工科技股份有限公司 | The cleansing and recycling method of containing benezene hydrogen chloride gas |
| CN112121603A (en) * | 2019-06-24 | 2020-12-25 | 万华化学集团股份有限公司 | Method and device for removing chlorobenzene from hydrogen chloride gas |
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