CN115138184A - Purification method of chlorination reaction tail gas and application thereof - Google Patents
Purification method of chlorination reaction tail gas and application thereof Download PDFInfo
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- CN115138184A CN115138184A CN202210879922.9A CN202210879922A CN115138184A CN 115138184 A CN115138184 A CN 115138184A CN 202210879922 A CN202210879922 A CN 202210879922A CN 115138184 A CN115138184 A CN 115138184A
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- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 58
- 238000000746 purification Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 132
- 239000007789 gas Substances 0.000 claims abstract description 71
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 47
- 238000001816 cooling Methods 0.000 claims description 27
- 238000004321 preservation Methods 0.000 claims description 20
- 238000007789 sealing Methods 0.000 claims description 14
- 238000009833 condensation Methods 0.000 claims description 12
- 230000005494 condensation Effects 0.000 claims description 12
- XEMRAKSQROQPBR-UHFFFAOYSA-N (trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=CC=C1 XEMRAKSQROQPBR-UHFFFAOYSA-N 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 7
- 239000002826 coolant Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 3
- 239000010815 organic waste Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000110 cooling liquid Substances 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- NPDACUSDTOMAMK-UHFFFAOYSA-N 4-Chlorotoluene Chemical compound CC1=CC=C(Cl)C=C1 NPDACUSDTOMAMK-UHFFFAOYSA-N 0.000 description 2
- CAHQGWAXKLQREW-UHFFFAOYSA-N Benzal chloride Chemical compound ClC(Cl)C1=CC=CC=C1 CAHQGWAXKLQREW-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical class C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003613 toluenes Chemical class 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1406—Multiple stage absorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1412—Controlling the absorption process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1418—Recovery of products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1487—Removing organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1493—Selection of liquid materials for use as absorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2045—Hydrochloric acid
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a purification method of chlorination reaction tail gas and application thereof, belonging to the technical field of chemical organic waste gas treatment and comprising a first washing device, a first circulating tank, a second washing device and a second circulating tank; s1, inputting chlorination reaction tail gas into a first washing device for primary washing, and inputting washed primary chlorination products into a first circulation tank for circular washing; s2, inputting the tail gas subjected to the primary washing into a second washing device, carrying out secondary washing, inputting the washed secondary chlorinated product into a second circulation tank, carrying out circulation washing, discharging the tail gas from the second washing device, entering a detection device, and discharging the tail gas out of the device after the tail gas is qualified; it can realize the recycle washing to prepare qualified hydrochloric acid for sale. The organic matter content in the hydrochloric acid is low, the hydrochloric acid purification treatment is not needed, the consumption of raw materials can be reduced, and the yield is improved by more than one percent.
Description
Technical Field
The invention relates to the technical field of chemical organic waste gas treatment, in particular to a purification method of chlorination reaction tail gas and application thereof.
Background
The side chain chlorination and ring chlorination of toluenes have the advantages of multiple reaction types, large production and wide application. At a certain reaction temperature, when the raw materials react with chlorine, hydrogen chloride gas is released, and organic matters such as the raw materials escape along with the hydrogen chloride gas to form reaction tail gas. The reaction tail gas is usually recovered by a multistage condensation recovery device. For example, when trichlorotoluene is produced by chlorination of toluene side chain, the tail gas contains organic matters such as raw material toluene, intermediate product monochlorotoluene, dichlorotoluene and the like besides a large amount of hydrogen chloride.
The method generally used for recovering organic substances in the reaction tail gas is as follows: firstly, water cooling recovery is carried out, and then freezing and deep cooling recovery is carried out; however, this method has the following problems in treating the exhaust gas:
1. because the hydrogen chloride is non-condensable gas, the gas still contains about 1 percent of organic matters although being recycled by multi-stage condensation; the tail gas enters a hydrochloric acid absorption system, the obtained hydrochloric acid contains organic matters, and the organic matters in the hydrochloric acid can be hydrolyzed or polymerized; for example, monochlorobenzene is hydrolyzed to generate benzyl alcohol, and biphenyl compounds are generated by polymerization, so that organic matters in hydrochloric acid are difficult to recycle.
2. Hydrochloric acid with high organic content cannot be directly sold as a byproduct, secondary pollution is caused, purification treatment is needed, and the common method comprises the following steps: a combination of methods such as settling separation, filtration, coalescence separation, resin adsorption, distillation, and the like; because hydrochloric acid has strong irritation, acidity and corrosivity, the purification equipment has high corrosion resistance and strong leakproofness, and the good operating environment is ensured; purifying by using hydrochloric acid after pretreatment and then by a resin adsorption method; however, more waste organic matters exist in the pretreatment, and when the resin is adsorbed, analyzed and regenerated, waste water and waste gas are generated, so that the organic matters can pollute the resin and reduce the service life of the resin; therefore, the investment of the purification equipment is large, the operation and maintenance cost is high, and the three wastes are generated more.
3. The reaction off-gas recovered by multi-stage condensation can be washed by a high boiling point washing agent, and the problems of how to recover organic matters dissolved in the washing agent and how to recycle the washing agent exist, so that the implementation is difficult.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a purification method of chlorination reaction tail gas and application thereof, which can realize recycling and washing to prepare qualified hydrochloric acid for sale. The organic matter content in the hydrochloric acid is low, the hydrochloric acid purification treatment is not needed, the consumption of raw materials can be reduced, and the yield is improved by more than one percent.
In order to solve the above problems, the present invention adopts the following technical solutions.
A purification method of chlorination reaction tail gas and application thereof are disclosed, which comprises a first washing device, a first circulating tank, a second washing device and a second circulating tank, wherein the first washing device is communicated with the second washing device through a gas pipeline, the first washing device is communicated with the first circulating tank through a first circulating pipeline, a first circulating pump for pressurization and a first cooling device for condensation temperature control are arranged between the first circulating pipelines, the second washing device is communicated with the second circulating tank through a second circulating pipeline, and a second circulating pump for pressurization and a second cooling device for condensation temperature control are arranged between the second circulating pipelines;
wherein the purification steps are as follows:
s1, inputting chlorination reaction tail gas into a first washing device for primary washing, inputting washed primary chlorination products into a first circulation tank for circulation washing;
s2, inputting the tail gas subjected to the primary washing into a second washing device, carrying out secondary washing, inputting the washed secondary chlorinated product into a second circulation tank, carrying out circulation washing, discharging the tail gas from the second washing device, entering a detection device, and discharging the tail gas out of the device after the tail gas is qualified;
s3, quantitatively adding fresh chlorinated materials into the second circulation tank, pressurizing by a set second circulation pump, condensing by a second cooling device, controlling the temperature, and inputting into a second washing device to serve as a secondary washing solution;
s4, inputting the secondary chlorination product washed by the second washing device into a first circulation tank, pressurizing by a circulation pump, inputting into a first cooling device for condensation temperature control, and finally inputting into the first washing device to serve as a primary washing solution;
s5, after cyclic washing, inputting the primary chlorination product of the first washing device into the chlorination reaction system again, and converting the raw material dissolved in the primary chlorination product into a product again; and meanwhile, inputting the secondary chlorination product of the second washing device into a hydrogen chloride absorption system to prepare qualified hydrochloric acid.
Further, the fresh chlorinated material is a fresh trichlorotoluene solution, the concentration of the fresh chlorinated material is 98%, and the primary washing liquid is a trichlorotoluene solution dissolved with 3-5% of organic matters.
Furthermore, the temperature of the first-stage washing liquid and the temperature of the second-stage washing liquid are both controlled within the range of 0-25 ℃.
Further, the spraying density of the first washing device and the second washing device is 30-100 m3/m2h.
Further, first washing device with second washing device structure size homogeneous phase is the same, and all includes the casing, casing bottom one side is provided with the air inlet, and the top is provided with the gas outlet, casing internally mounted has the whirl board, the whirl board top is provided with the liquid deconcentrator.
Furthermore, the liquid disperser with the whirl plate be provided with three groups at least in the casing, and install the filler between adjacent each group, the inside top of casing is installed the defroster.
Further, the filler is ceramic, graphite or tetrafluoro filler.
Further, the casing bottom still be provided with the leakage fluid dram that first circulation groove and second circulation groove are linked together, gas-liquid separator is installed to leakage fluid dram port department.
Further, first cooling device with second cooling device structure size homogeneous phase is the same, and all includes the heat preservation shell, installs in the sealing top cap on heat preservation shell top and installs in the sealed bottom of heat preservation shell bottom, the heat preservation shell is inside to have the heat exchange tube through being provided with top closing plate and bottom closing plate fixed mounting, heat preservation shell bottom one side is provided with the inlet, and top one side is provided with the liquid outlet, sealing top cap center is provided with the division board, and wherein one side is provided with the coolant liquid export, and the opposite side is provided with the coolant liquid import.
Furthermore, baffle plates are welded between the heat exchange tubes and the inner wall of the heat preservation shell in an equidistant and staggered mode, and the baffle plates are of a three-quarter disc-shaped structure.
Compared with the prior art, the invention has the advantages that:
(1) According to the scheme, the first washing device and the second washing device are used as main removing equipment, organic matters in chlorination reaction tail gas are circularly washed and absorbed through chlorination products, so that the content of the organic matters in the secondary chlorination products is low, the secondary chlorination products are input into a hydrogen chloride absorption system, qualified hydrochloric acid can be prepared and sold, the content of the organic matters in the hydrochloric acid is low, and the hydrochloric acid does not need to be purified.
(2) This scheme is with first washing device and second washing device cooperation, can go in directly importing the first-class chlorination product of output to chlorination for the volatile raw materials in the tail gas, monochlorotoluene, dichlorotoluene intermediate are circulated washing absorption by the chlorination product, can all turn into the product, reduce the quantity of raw materials, improve the product yield.
(3) The scheme circularly washes and absorbs the chlorination product, and simultaneously absorbs other harmful substances in the tail gas by using materials such as ceramics, graphite, tetrafluoro and the like, and has the advantages of simple equipment, investment saving and stable operation.
(4) This scheme utilization whirl board and liquid deconcentrator cooperate for chlorination tail gas resistance that rises is less, and then can not cause the resistance increase of system because of washing, thereby has avoided reaction system easily to take place to leak, influences the problem of environment and equipment corrosion, and whirl board and liquid deconcentrator cooperate washing liquid and chlorination reaction tail gas to realize abundant contact simultaneously, and then make the organic matter dissolve more fully, thereby guarantee the tail gas treatment efficiency of this system.
Drawings
FIG. 1 is a schematic diagram of a purification system according to the present invention;
FIG. 2 is a schematic diagram of the circulation structure of the purification system of the present invention;
FIG. 3 is a schematic structural view of a first washing device and a second washing device according to the present invention;
fig. 4 is a schematic structural diagram of a first cooling device and a second cooling device of the present invention.
The reference numbers in the figures illustrate:
1. a first washing device; 101. a housing; 102. an air inlet; 103. an air outlet; 104. a demister; 105. a filler; 106. a liquid disperser; 107. a swirl plate; 108. a liquid discharge port; 109. a gas-liquid separator; 2. a first circulation tank; 3. a second washing device; 4. a second circulation tank; 5. a first cooling device; 501. a heat preservation shell; 502. sealing the top cover; 503. sealing the bottom cover; 504. a heat exchange pipe; 505. a top seal plate; 506. a bottom seal plate; 507. a separator plate; 508. a coolant outlet; 509. a coolant inlet; 510. a liquid outlet; 511. a liquid inlet; 512. a baffle plate; 6. circulating a pump; 7. a second cooling device; 8. a second circulating pump; 9. a chlorination reaction system; 10. a hydrogen chloride absorption system.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
The embodiment is as follows:
referring to fig. 1-4, a purification method of chlorination reaction tail gas and an application thereof include a first washing device 1, a first circulation tank 2, a second washing device 3 and a second circulation tank 4, wherein the first washing device 1 and the second washing device 3 are communicated through a gas pipeline, the first washing device 1 and the first circulation tank 2 are communicated through a first circulation pipeline, a first circulation pump 6 for pressurization and a first cooling device 5 for condensation temperature control are arranged between the first circulation pipelines, the second washing device 3 and the second circulation tank 4 are communicated through a second circulation pipeline, and a second circulation pump 8 for pressurization and a second cooling device 7 for condensation temperature control are arranged between the second circulation pipelines;
wherein the purification steps are as follows:
s1, inputting chlorination reaction tail gas into a first washing device 1 for primary washing, inputting washed primary chlorination products into a first circulation tank 2 for circulation washing;
s2, inputting the tail gas subjected to the primary washing into a second washing device 3, carrying out secondary washing, inputting the washed secondary chlorinated product into a second circulating tank 4, carrying out circulating washing, discharging the tail gas from the second washing device 3, entering a detection device, and discharging the tail gas out of the device after the tail gas is qualified;
s3, quantitatively adding fresh chlorinated materials into the second circulation tank 4, pressurizing by a second circulation pump 8, condensing by a second cooling device 7, controlling the temperature, and inputting into the second washing device 3 to serve as a secondary washing solution;
s4, inputting the secondary chlorination product washed by the second washing device 3 into the first circulating tank 2, pressurizing by a circulating pump 6, inputting into a first cooling device 5 for condensation temperature control, and finally inputting into the first washing device 1 to serve as a primary washing liquid;
s5, after the cyclic washing, inputting the primary chlorination product of the first washing device 1 into the chlorination reaction system 9 again, and converting the raw material dissolved in the primary chlorination product into a product again; meanwhile, the secondary chlorination product of the second washing device 3 is input into a hydrogen chloride absorption system 10 to prepare qualified hydrochloric acid.
Referring to fig. 1 and fig. 2, the fresh chlorinated material is a fresh trichlorotoluene solution with a concentration of 98%, and the primary washing liquid is a trichlorotoluene solution in which organic matters in the chlorination tail gas are dissolved.
Referring to fig. 1 and fig. 2, the temperature of the primary washing liquid and the secondary washing liquid is controlled within the range of 0 to 25 ℃, in this embodiment, 12 ℃ is selected, in the washing process, the washing removal rate of volatile materials such as toluene in the tail gas is directly related to the washing temperature, the washing temperature is high, the removal rate is low, but the freezing point of trichlorotoluene is below-7 ℃, and trichlorotoluene is solidified at too low temperature; the temperature of the chlorination reaction tail gas after freezing and deep cooling is about minus 5 ℃, the temperature of trichlorotoluene feeding is kept below 25 ℃, and the washing efficiency can be ensured.
Referring to fig. 1 and 2, the spraying density of the first washing device 1 and the second washing device 3 is 30-100 m3/m2h, and 60m3/m2h is selected in this embodiment, so that the washing effect of the first washing device 1 and the second washing device 3 can be ensured, in addition, the circulation amount of the washing liquid at each stage is also an important operating parameter, the spraying washing amount is small, the contact area between the gas and the washing liquid is small, and the washing effect is reduced, so that the spraying density of the first washing device 1 and the second washing device 3 needs to be controlled according to the washing effect.
Referring to fig. 3, the first washing device 1 and the second washing device 3 are identical in structure and size, and both include a housing 101, an air inlet 102 is disposed on one side of the bottom end of the housing 101, and an air outlet 103 is disposed on the top end of the housing 101, a swirl plate 107 is mounted inside the housing 101, a liquid disperser 106 is disposed on the top end of the swirl plate 107, at least three groups of liquid dispersers 106 and swirl plates 107 are disposed inside the housing 101, tail gas can be input into the housing 101 through the air inlet 102, washing liquid is input through the liquid disperser 106 and dispersed in a spraying manner, the spraying density is 60m3/m2h, air flow passes through the swirl plate 107, the swirl plate 107 is driven to rotate by thrust of ascending air flow, so that the tail gas input by the washing liquid is fully contacted, sufficient absorption of organic matters is ensured, and fillers 105 are mounted between adjacent groups, other harmful substances in the tail gas can be absorbed, meanwhile, a demister 104 is mounted on the top end inside the housing 101, and discharge amount of vaporized liquid carried by the air flow can be reduced.
Referring to fig. 3, wherein the filler 105 is a ceramic, graphite, or teflon filler.
Referring to fig. 3, the bottom end of the casing 101 is further provided with a liquid outlet 108 communicated with the first circulation tank 2 and the second circulation tank 4 for discharging the washed chlorinated product, and a gas-liquid separator 109 is installed at a port of the liquid outlet 108 for separating gas and liquid to prevent the tail gas from leaking.
Referring to fig. 4, the first cooling device 5 and the second cooling device 7 have the same structure and size, and each of the first cooling device and the second cooling device includes a heat preservation casing 501, a top sealing cover 502 mounted on the top end of the heat preservation casing 501, and a bottom sealing cover 503 mounted on the bottom end of the heat preservation casing 501, a heat exchange tube 504 is fixedly mounted inside the heat preservation casing 501 through a top sealing plate 505 and a bottom sealing plate 506, a liquid inlet 511 is disposed on one side of the bottom end of the heat preservation casing 501, a liquid outlet 510 is disposed on one side of the top end, a partition plate 507 is disposed in the center of the top sealing cover 502, a cooling liquid outlet 508 is disposed on one side of the top sealing cover, and a cooling liquid inlet 509 is disposed on the other side of the top sealing cover, and the cooling liquid enters the heat exchange tube 504 near the one side of the heat preservation casing and enters the heat exchange tube 504 near the other side of the top sealing cover 503, and is discharged from the cooling liquid outlet 508, and the cooling liquid enters the casing 101 through the liquid inlet 511 and fully contacts with the heat exchange tube 504, and is finally discharged from the liquid outlet 510, so that the washing liquid is at a desired temperature.
Referring to fig. 4, the baffle plates 512 are welded between the heat exchange tubes 504 and the inner wall of the heat preservation shell 501 in an equidistant and staggered manner, and the baffle plates 512 are in a three-quarter disc-shaped structure, so that the flow velocity of the cleaning solution can be reduced in the flowing process of the cleaning solution, and the cleaning solution can flow in a bent manner, so that the contact area between the cleaning solution and the heat exchange tubes 504 can be increased, and the heat exchange efficiency can be improved.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (10)
1. The utility model provides a purification device of chlorination tail gas, includes first washing device (1), first circulation groove (2), second washing device (3) and second circulation groove (4), its characterized in that: first washing device (1) with be linked together through being provided with gas piping between second washing device (3), first washing device (1) with be linked together through being provided with first circulating line between first circulating tank (2), just be provided with between the first circulating line and be used for the first cooling device (5) of pressurized circulation pump (6) and be used for the condensation accuse temperature, second washing device (3) with be linked together through being provided with the second circulating line between second circulating tank (4), be provided with between the second circulating line and be used for pressurized circulation secondary pump (8) and be used for second cooling device (7) of condensation accuse temperature.
2. The purification device of the chlorination reaction tail gas of claim 1, wherein: first washing device (1) with second washing device (3) structure size homogeneous phase, and all include casing (101), casing (101) bottom one side is provided with air inlet (102), and the top is provided with gas outlet (103), casing (101) internally mounted has whirl board (107), whirl board (107) top is provided with liquid disperser (106).
3. The device for purifying the chlorination reaction tail gas according to claim 2, wherein: the liquid disperser (106) and the swirl plate (107) are at least provided with three groups in the shell (101), a filler (105) is arranged between each adjacent group, the top end in the shell (101) is provided with a demister (104), and the filler (105) is ceramic, graphite or tetrafluoro filler.
4. The device for purifying the chlorination reaction tail gas according to claim 3, wherein: casing (101) bottom still be provided with drain outlet (108) that first circulation groove (2) and second circulation groove (4) are linked together, gas-liquid separator (109) are installed to drain outlet (108) port department.
5. The purification device of the chlorination reaction tail gas of claim 1, wherein: first cooling device (5) with second cooling device (7) structure size is the same, and all includes heat preservation shell (501), installs in sealed top cap (502) on heat preservation shell (501) top and installs in sealed bottom (503) of heat preservation shell (501) bottom, heat preservation shell (501) inside through being provided with top sealing plate (505) and bottom sealing plate (506) fixed mounting have heat exchange tube (504), heat preservation shell (501) bottom one side is provided with inlet (511), and top one side is provided with liquid outlet (510), sealed top cap (502) center is provided with division board (507), and wherein one side is provided with coolant liquid export (508), and the opposite side is provided with coolant liquid import (509).
6. The device for purifying the chlorination reaction tail gas according to claim 5, wherein: baffle plates (512) are welded between the heat exchange tubes (504) and the inner wall of the heat preservation shell (501) in an equidistant and staggered mode, and the baffle plates (512) are of a three-quarter disc-shaped structure.
7. A purification method of chlorination reaction tail gas is characterized in that: the purification device applied to the tail gas of the chlorination reaction of any one of the claims 1-6, comprising the following steps:
s1, inputting chlorination reaction tail gas into a first washing device (1) for primary washing, and inputting a washed primary chlorination product into a first circulating tank (2) for circulating washing;
s2, inputting the tail gas subjected to the primary washing into a second washing device (3), carrying out secondary washing, inputting the secondary chlorinated product after washing into a second circulating tank (4), carrying out circulating washing, discharging the tail gas from the second washing device (3), entering a detection device, and discharging the tail gas out of the device after the tail gas is qualified;
s3, quantitatively adding fresh chlorinated materials into the second circulation tank (4), pressurizing by a second circulation pump (8), condensing by a second cooling device (7) to control the temperature, and inputting into the second washing device (3) to serve as a secondary washing solution;
s4, inputting the secondary chlorination product washed by the second washing device (3) into the first circulation tank (2), pressurizing by a circulation pump (6), inputting into a first cooling device (5) for condensation temperature control, and finally inputting into the first washing device (1) to serve as a primary washing solution;
s5, after cyclic washing, inputting the primary chlorination product of the first washing device (1) into the chlorination reaction system (9) again, and converting the raw material dissolved in the primary chlorination product into a product again; meanwhile, the secondary chlorination product of the second washing device (3) is input into a hydrogen chloride absorption system (10) to prepare qualified hydrochloric acid.
8. The purification method of chlorination reaction tail gas according to claim 7, wherein: the fresh chlorinated material is a fresh trichlorotoluene solution, the concentration of the fresh chlorinated material is 98%, and the primary washing liquid is a trichlorotoluene solution dissolved with 3-5% of organic matters.
9. The method for purifying the chlorination reaction tail gas according to claim 7, wherein the method comprises the following steps: the temperature of the first-stage washing liquid and the temperature of the second-stage washing liquid are both controlled within the range of 0-25 ℃, and the spraying density of the first washing device (1) and the second washing device (3) is 30-100 m3/m2h.
10. The application of the purification method of chlorination reaction tail gas is characterized in that: the method is applied to the chlorination reaction tail gas treatment.
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