CN113398719A - Device and method for recovering chlorine in tail chlorine - Google Patents
Device and method for recovering chlorine in tail chlorine Download PDFInfo
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- CN113398719A CN113398719A CN202110661074.XA CN202110661074A CN113398719A CN 113398719 A CN113398719 A CN 113398719A CN 202110661074 A CN202110661074 A CN 202110661074A CN 113398719 A CN113398719 A CN 113398719A
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 239000000460 chlorine Substances 0.000 title claims abstract description 154
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 154
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000003795 desorption Methods 0.000 claims abstract description 92
- 238000010521 absorption reaction Methods 0.000 claims abstract description 90
- 239000002904 solvent Substances 0.000 claims abstract description 51
- 239000000463 material Substances 0.000 claims abstract description 37
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003513 alkali Substances 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 19
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 62
- 239000007789 gas Substances 0.000 claims description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000945 filler Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 238000012856 packing Methods 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 14
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 229950005499 carbon tetrachloride Drugs 0.000 claims description 5
- 229960001701 chloroform Drugs 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 3
- 239000010962 carbon steel Substances 0.000 claims description 3
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 claims description 2
- -1 and more preferably Substances 0.000 claims description 2
- 150000001805 chlorine compounds Chemical group 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 229950011008 tetrachloroethylene Drugs 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002699 waste material Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229960002089 ferrous chloride Drugs 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 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
- BCBIXNWEWWQJST-UHFFFAOYSA-N ClICl Chemical compound ClICl BCBIXNWEWWQJST-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- FWMUJAIKEJWSSY-UHFFFAOYSA-N sulfur dichloride Chemical compound ClSCl FWMUJAIKEJWSSY-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 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
-
- 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
- B01D53/002—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 condensation
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0743—Purification ; Separation of gaseous or dissolved chlorine
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
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- Chemical & Material Sciences (AREA)
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- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention belongs to the technical field of chlor-alkali production, and particularly relates to a device and a method for recovering chlorine in tail chlorine. The method for recovering chlorine in tail chlorine comprises the steps of solvent absorption, solvent desorption, liquid chlorine storage and tail gas treatment, wherein the solvent absorption is carried out in an absorption tower in a device, tail gas which is not absorbed by the solvent is discharged after sequentially passing through an absorption tower condenser, a tail gas alkali washing tower and an incineration device, the solvent which absorbs the chlorine flows out of the bottom of the absorption tower, is heated by a material heat exchanger and then enters a desorption tower for desorption, the desorbed chlorine is condensed by a desorption tower cooler and enters a liquid chlorine storage tank, and the desorbed solvent is re-returned to the absorption tower for recycling through the material heat exchanger and the cooler. The chlorine recovery rate of the invention reaches 99.9%, the solvent can be recycled, the solvent treatment cost is reduced, the economic benefit of enterprises is improved, and the generated tail gas is discharged after alkali washing and incineration, thereby reducing the pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of chlor-alkali production, and particularly relates to a device and a method for recovering chlorine in tail chlorine.
Background
The chlor-alkali industry refers to the industry that produces sodium hydroxide solution, chlorine and hydrogen by electrolyzing sodium chloride solution and uses them as raw materials, and tail chlorine is inevitably generated in production, if the waste chlorine can not be processed in time and is directly discharged into the air, air pollution is caused, and when the mass concentration of the waste chlorine is accumulated to a certain value, explosion accidents are possibly caused. At present, the methods for absorbing and recycling chlorine at home and abroad mainly comprise a synthetic hydrochloric acid method, a solvent absorption method, a liquid chlorine production method, an alkali liquor absorption method, a sodium sulfite absorption method, a ferrous chloride absorption method and the like.
The synthetic hydrochloric acid method is that chlorine in tail gas is purified to remove impurities such as dust, and then reacts with hydrogen to generate hydrogen chloride gas, and then the hydrogen chloride gas is sprayed by water or absorbed by water to form hydrochloric acid as a byproduct. The method has mature process and simple equipment, but the purity of the chlorine in the tail gas usually hardly meets the requirement of synthesizing the hydrochloric acid. When the process is used for treating chlorine-containing tail gas, high-purity hydrogen is often needed to be supplemented, so that the amount of hydrochloric acid as a byproduct is large, the quality is not high, and the treatment cost of the tail gas is high, so that the process is rarely adopted.
The alkali liquor absorption method is the main method for treating chlorine-containing waste gas currently in China, and the absorbent comprises alkaline aqueous solution or slurry of sodium hydroxide, sodium carbonate, calcium hydroxide and the like. During the absorption process, the alkaline absorbent effectively converts chlorine in the exhaust gas to hypochlorite as a by-product. The method has the advantages of mature and reliable technology and low investment, and is widely used for treating chlorine-containing tail gas. Although the alkali solution absorption method is widely used, the operation cost is high, secondary pollution is generated when hypochlorite cannot be sold as a product, and in order to avoid the secondary pollution, a chlorine treatment process of adding sulfite into an alkaline solution as an absorption solution is also adopted. For example, the chlorine in the tail gas is circularly absorbed by adopting a mixed solution of sodium sulfite and sodium hydroxide, and the method is similar to the conventional alkali liquor absorption process and has reliable technology; but the production control is relatively complicated, the operation cost is high, and the added value of the generated sulfate is very low.
The ferrous chloride absorption method usually needs to add waste scrap iron, the ferrous chloride is oxidized into ferric chloride, ferric iron can be reduced into ferrous iron again due to the existence of the scrap iron, waste chlorine is continuously introduced, the ferrous iron is oxidized into ferric iron, and the circular absorption of the chlorine is realized. The process for treating waste chlorine by using waste iron filings has the advantages of low required cost, simple method and cyclic absorption and utilization, but the products are ferric chloride and ferric oxide, so that the problems of short supply and rising price of industrial chlorine cannot be solved.
The solvent absorption method is to wash chlorine-containing waste gas with an organic or inorganic solvent, the solvent absorbs the chlorine gas therein, then pure chlorine gas is desorbed by heating or pressurizing, and the desorbed solvent is recycled, or the chlorine-containing solvent is used as a production raw material in the production process. The common solvents include benzene, sulfur dichloride, carbon tetrachloride, chlorosulfonic acid, iodine dichloride aqueous solution, etc. Although the practical history of chlorine recovery by a solvent absorption method is long, the process is simple and is always the subject of deep research in the chlor-alkali chemical industry, and although carbon tetrachloride is used for enriching and extracting chlorine at present, the recovery rate is generally low, and the industrial requirements of high recovery rate and high economic benefit cannot be met.
U.S. Pat. No. 5,5861049 (application No. US08898566) discloses a process for recovering chlorine from tail chlorine by a combination of condensation, flash evaporation and membrane separation, wherein chlorine in the tail chlorine is first condensed into liquid chlorine at low temperature and high pressure, the liquid chlorine is flashed to remove low boiling point gas components, and the uncondensed chlorine is recovered by the membrane separation technique, but the patent only concentrates chlorine at a yield of 80% at most by condensation, and the total yield can reach 98% by subsequent membrane separation, and the process for recovering chlorine is complex and has higher cost.
Disclosure of Invention
The tail chlorine refers to waste gas generated in the chlor-alkali industry and containing a large amount of chlorine, wherein the chlorine can cause serious air pollution and resource waste if being directly discharged without being treated. The invention provides a device and a method for recovering chlorine from tail chlorine, aiming at solving the problems of low chlorine recovery rate, high cost and complex process in tail chlorine in the chlor-alkali industry.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for recovering chlorine in tail chlorine, which comprises the following steps of solvent absorption, solvent desorption, liquid chlorine storage and tail gas treatment:
solvent absorption: tail chlorine from a chlor-alkali plant enters the lower part of the absorption tower, and the solvent is sprayed from the upper part of the absorption tower, wherein the volume flow of the tail chlorine is 500-600Nm3The mass flow rate of the solvent is 20-24T/h;
and (3) solvent desorption: discharging the solvent for absorbing chlorine from the bottom of the absorption tower, preheating the solvent, then desorbing the preheated solvent in a desorption tower, cooling the desorbed solution, refluxing the cooled solution, recycling the solution in the absorption tower, and storing the chlorine obtained by desorption;
liquid chlorine storage: condensing the chlorine obtained by desorption and then storing the chlorine in a liquid chlorine storage tank;
tail gas treatment: tail chlorine which is not absorbed by the solvent in the absorption tower is discharged after condensation, alkali liquor absorption and incineration in sequence.
Preferably, the tail chlorine comprises, in volume fraction: 60-80% of chlorine gas, 20-40% of air and trace hydrogen, and further preferably, the tail chlorine comprises the following components in percentage by volume: 70% of chlorine, 29.8% of air and 0.2% of hydrogen.
Preferably, the solvent is a chloride such as dichloromethane, chloroform, carbon tetrachloride, and tetrachloroethylene, and more preferably, the solvent is carbon tetrachloride.
Preferably, the temperature of the absorption column is-15 to 0 ℃ and the pressure is 0 to 0.05MPa (P), more preferably 0 to 0.02MPa (P), wherein (P) is a gauge pressure.
Preferably, the ratio of the volume flow of tail chlorine absorbed by the solvent to the mass flow of the solvent is 125 (5-6) Nm3/T。
Preferably, the pressure of the desorption tower is 0.3-0.4MPa (P), the temperature at the top of the tower is 0-10 ℃, the temperature at the bottom of the tower is 125-135 ℃, and further preferably, the temperature at the top of the tower is 0-5 ℃ and the temperature at the bottom of the tower is 128-132 ℃.
The invention also provides a device for recovering chlorine in tail chlorine, which comprises an absorption circulation unit, a desorption unit, a storage unit and a tail gas treatment unit, wherein one end of the absorption circulation unit is sequentially connected with the desorption unit and the storage unit, and the other end of the absorption circulation unit is connected with the tail gas treatment unit;
the absorption circulation unit comprises an absorption tower, a carbon tetrachloride circulation pump, a material heat exchanger, a cooler and an absorption tower condenser, wherein a foam cover layer positioned on the upper layer and a packing layer positioned on the lower layer are arranged in the absorption tower; the tower bottom of the absorption tower is connected with a low-temperature inlet of a material heat exchanger through a carbon tetrachloride circulating pump, a low-temperature outlet of the material heat exchanger is connected with a first-stage cooler, a high-temperature outlet is connected with a high-temperature inlet and a desorption unit, the third-stage cooler is respectively connected with an upper reflux inlet and a middle reflux inlet of the absorption tower, the upper reflux inlet is arranged above the bubble cap layer, and the middle reflux inlet is arranged above the packing layer and below the bubble cap layer;
the desorption unit comprises a desorption tower, a desorption tower material pump and a desorption tower reboiler; the high-temperature outlet of the material heat exchanger is connected with the middle part of the desorption tower, the bottom of the desorption tower is connected with the high-temperature inlet of the material heat exchanger through a desorption tower material pump, the bottom of the desorption tower is connected with a desorption tower reboiler, and the top of the desorption tower is connected with a storage unit;
the storage unit comprises a desorption tower cooler and a liquid chlorine storage tank, wherein the desorption tower cooler is a carbon steel tubular heat exchanger; the top of the desorption tower is connected with a liquid chlorine storage tank through a desorption tower cooler;
the tail gas treatment unit comprises a tail gas alkaline washing tower and an incineration device; one end of the tail gas alkaline washing tower is connected with the top of the absorption tower through an absorption tower condenser, and the other end of the tail gas alkaline washing tower is connected with the incineration device.
Preferably, the blister layer comprises 5-7 layers of blisters, further preferably, the blister layer comprises 6 layers of blisters, the filler layer comprises 6-12 meters of filler, further preferably, the filler layer comprises 8 meters of filler, and the filler is stainless steel mesh filler CY 700.
Preferably, the desorption tower is a packed tower, and the packing of the desorption tower is stainless steel wire mesh packing CY 700.
Preferably, the working pressure of the liquid chlorine storage tank is 0.3-0.4MPa, and the tail gas alkaline washing tower is filled with alkaline liquor, wherein the alkaline liquor is NaOH solution with the mass fraction of 10%.
The devices are connected through pipelines.
One or more technical solutions provided by the embodiments of the present invention have at least the following technical effects:
(1) the invention recovers the chlorine from the tail chlorine by utilizing the difference that the chlorine in the tail chlorine has very high solubility in the solvent and the solubilities of other components are very low, and the recovery rate reaches 99.9 percent.
(2) The components which are not recovered in the method are incinerated by the incinerating device after passing through the tail gas alkali washing tower, so that the pollution of tail gas emission to the environment is avoided.
(3) The solvent adopted in the invention can be recycled, and the chlorine in the tail gas can be repeatedly absorbed, thereby reducing the solvent treatment cost, improving the chlorine recovery rate and improving the economic benefit of enterprises.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Wherein, 1, an absorption tower; 2. a carbon tetrachloride circulating pump; 3. a material heat exchanger; 30. a cooler; 31. a low temperature inlet; 32. a high temperature outlet; 33. a high temperature inlet; 34. a low temperature outlet; 4. a primary cooler; 5. a secondary cooler; 6. a tertiary cooler; 7. an absorption tower condenser; 81. a tail gas alkaline washing tower; 82. an incineration device; 9. a desorber material pump; 10. a desorption tower; 11. a desorber reboiler; 12. a desorber cooler; 13. a liquid chlorine storage tank; 14. a blister layer; 15. a filler layer; 16. an upper return inlet; 17. and the middle part is provided with a backflow inlet.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
It should be noted that the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents, materials and equipment are commercially available, unless otherwise specified.
Example 1
A device for recovering chlorine from tail chlorine comprises an absorption circulation unit, a desorption unit, a storage unit and a tail gas treatment unit, wherein one end of the absorption circulation unit is sequentially connected with the desorption unit and the storage unit, and the other end of the absorption circulation unit is connected with the tail gas treatment unit;
the absorption circulation unit comprises an absorption tower 1, a carbon tetrachloride circulation pump 2, a material heat exchanger 3, a cooler 30 and an absorption tower condenser 7, a foam cover layer 14 positioned on the upper layer and a filler layer 15 positioned on the lower layer are arranged in the absorption tower 1, the cooler 30 comprises a first-stage cooler 4, a second-stage cooler 5 and a third-stage cooler 6 which are connected in series, the material heat exchanger 3 comprises a low-temperature inlet 31, a high-temperature outlet 32, a high-temperature inlet 33 and a low-temperature outlet 34, and the top of the absorption tower 1 is connected with a tail gas treatment unit through the absorption tower condenser 7; the tower bottom of the absorption tower 1 is connected with a low-temperature inlet 31 of a material heat exchanger 3 through a carbon tetrachloride circulating pump 2, a low-temperature outlet 34 of the material heat exchanger 3 is connected with a first-stage cooler 4, a high-temperature outlet 32 is connected with a high-temperature inlet 33 to form a desorption unit, a third-stage cooler 6 is respectively connected with an upper reflux inlet 16 and a middle reflux inlet 17 of the absorption tower 1, the upper reflux inlet 16 is arranged on the upper portion of the foam cover layer 14, and the middle reflux inlet 17 is arranged on the upper portion of the packing layer.
The desorption unit comprises a desorption tower 10, a desorption tower material pump 9 and a desorption tower reboiler 11; the high-temperature outlet 32 of the material heat exchanger 3 is connected with the middle part of the desorption tower 10, the bottom of the desorption tower 10 is connected with the high-temperature inlet 33 of the material heat exchanger 3 through a desorption tower material pump 9, the bottom of the desorption tower 10 is connected with a desorption tower reboiler 11, and the top of the desorption tower is connected with a storage unit;
the storage unit comprises a desorption tower cooler 12 and a liquid chlorine storage tank 13, wherein the desorption tower cooler 12 is a carbon steel tube-in-tube heat exchanger; the top of the desorption tower 10 is connected with a liquid chlorine storage tank 13 through a desorption tower cooler 12;
the tail gas treatment unit comprises a tail gas alkaline washing tower 81 and an incineration device 82; one end of the tail gas alkaline washing tower 81 is connected with the top of the absorption tower 1 through the absorption tower condenser 7, and the other end is connected with the burning device 82.
The devices are connected through pipelines.
The blister layer 14 comprises 6 layers of blisters, the filler layer comprises 8 metres of filler, and the filler is stainless steel mesh filler CY 700.
The desorption tower 10 is a packed tower, and the packing is stainless steel wire mesh packing CY 700.
The working pressure of the liquid chlorine storage tank is 0.3-0.4Mpa (P), and NaOH solution with the mass fraction of 10% is contained in the tail gas alkaline washing tower.
Comparative example 1
The device for recovering chlorine gas from tail chlorine is characterized in that an absorption tower 1 is a bubble cap tower, bubble caps are 6 layers, and the rest of the structure and the connection relation are the same as those of the embodiment 1.
Comparative example 2
The device for recovering chlorine from tail chlorine is characterized in that an absorption tower 1 is a packed tower, the packing is 10 meters, and the rest of the structure and the connection relation are the same as those of the embodiment 1.
Example 2
A method for recovering chlorine gas from tail chlorine, comprising the steps of:
the process was carried out using the apparatus of example 1, comparative example 1 and comparative example 2, respectively, with tail chlorine having the composition of 70% chlorine, 29.8% air, 0.2% hydrogen at a flow rate of 500Nm from a chlor-alkali plant3h enters the bottom of an absorption tower 1, is in contact mass transfer with carbon tetrachloride sprayed by the absorption tower 1 at the temperature of minus 10 ℃ and the flow rate of 20T/h, chlorine in tail chlorine is absorbed and then flows out of the tower kettle of the absorption tower 1 together with the carbon tetrachloride, passes through a material heat exchanger 3, the temperature is raised to 60 ℃ and then enters the middle part of a desorption tower 10, the chlorine is heated and separated from the carbon tetrachloride, the pressure of the desorption tower 10 is controlled to be 0.3MPa (P), the kettle temperature is 130 ℃, the chlorine is desorbed from the top of the desorption tower 10 and then enters a liquid chlorine storage tank 13 through a desorption tower cooler 12, the carbon tetrachloride is extracted from the tower kettle 10 of the desorption tower, and then continues to enter the absorption tower 1 after sequentially passing through the material heat exchanger 3, a primary cooler 4, a secondary cooler 5 and a tertiary cooler 6 and being cooled to the temperature of 80 ℃, the temperature of 40 ℃, the temperature of 15 ℃ and the temperature of-10 ℃, in the apparatus of example 1, a portion of the refluxed carbon tetrachloride was fed at a flow rate of 19T/h.Into the filler layer and the other part into the foam layer at a flow rate of 1T/h. The volume fractions of the absorbed tail gas components air/hydrogen/chlorine are shown in table 1, and the tail gas enters a tail gas alkaline washing tower 81 to remove chlorine and then enters an incineration device 82 for incineration. Chlorine recovery is shown in table 2.
TABLE 1 composition of tail gas under different apparatus and process conditions
Example 3
A method for recovering chlorine gas from tail chlorine, comprising the steps of:
the process was carried out using the apparatus of example 1, comparative example 1 and comparative example 2, respectively, with tail chlorine having the composition of 70% chlorine, 29.8% air, 0.2% hydrogen at a flow rate of 600Nm from a chlor-alkali plant3The chlorine in the tail chlorine is absorbed and flows out of the tower kettle together with the carbon tetrachloride after being absorbed, the chlorine passes through the material heat exchanger 3, the temperature is raised to 60 ℃ and then enters the middle part of the desorption tower 10, the chlorine is heated and is separated from the carbon tetrachloride, the pressure of the desorption tower is controlled to be 0.3MPa (P), the kettle temperature is 130 ℃, the chlorine is desorbed from the tower top and is condensed by the desorption tower cooler 12 to enter the liquid chlorine storage tank 13, the carbon tetrachloride is extracted from the tower kettle, the chlorine continues to enter the absorption tower 1 after sequentially passing through the material heat exchanger 3, the primary cooler 4, the secondary cooler 5 and the tertiary cooler 6 to be cooled to 80 ℃, 40 ℃, 15 ℃ and 10 ℃, and in the device of the embodiment 1, one part of the refluxed carbon tetrachloride enters the packing layer with the flow rate of 23T/h, the other part enters the bubble cap layer at a flow rate of 1T/h. The volume fractions of the absorbed tail gas components air/hydrogen/chlorine are shown in table 1, and the tail gas enters a tail gas alkaline washing tower 81 to remove chlorine and then enters an incineration device 82 for incineration. Chlorine recovery is shown in table 2.
Example 4
A method for recovering chlorine gas from tail chlorine, comprising the steps of:
the process was carried out using the apparatus of example 1, comparative example 1 and comparative example 2, respectively, with a composition of 70% chlorineTail chlorine of gas, 29.8% air, 0.2% hydrogen from chlor-alkali plant at a flow rate of 500Nm3The chlorine in the tail chlorine is absorbed and flows out of the tower kettle together with the carbon tetrachloride after being absorbed, the chlorine passes through the material heat exchanger 3, the temperature is raised to 60 ℃ and then enters the middle part of the desorption tower 10, the chlorine is heated and is separated from the carbon tetrachloride, the pressure of the desorption tower is controlled to be 0.3MPa (P), the kettle temperature is 130 ℃, the chlorine is desorbed from the tower top and is condensed by the desorption tower cooler 12 to enter the liquid chlorine storage tank 13, the carbon tetrachloride is extracted from the tower kettle, the chlorine continues to enter the absorption tower 1 after sequentially passing through the material heat exchanger 3, the primary cooler 4, the secondary cooler 5 and the tertiary cooler 6 to be cooled to 80 ℃, 40 ℃, 15 ℃ and 10 ℃, and in the device of the embodiment 1, one part of the refluxed carbon tetrachloride enters the packing layer with the flow rate of 23T/h, the other part enters the bubble cap layer at a flow rate of 1T/h. The volume fractions of the absorbed tail gas components air/hydrogen/chlorine are shown in table 1, and the tail gas enters a tail gas alkaline washing tower 81 to remove chlorine and then enters an incineration device 82 for incineration. Chlorine recovery is shown in table 2.
Example 5
A method for recovering chlorine gas from tail chlorine, comprising the steps of:
the process was carried out using the apparatus of example 1 and the gas-to-liquid flow ratio of example 4, with tail chlorine having the composition of 70% chlorine, 29.8% air, 0.2% hydrogen at a flow rate of 500Nm from a chlor-alkali plant3h enters the bottom of an absorption tower 1, is contacted with trichloromethane sprayed by the absorption tower 1 at the temperature of minus 10 ℃ and with the flow rate of 24T/h for mass transfer, chlorine in tail chlorine flows out of a tower kettle together with the trichloromethane after being absorbed, passes through a material heat exchanger 3, enters the middle part of a desorption tower 10 after the temperature is raised to 60 ℃, is heated to be separated from the trichloromethane, controls the pressure of the desorption tower to be 0.3MPa (P), has the kettle temperature of 130 ℃, is desorbed from the top of the tower, passes through a desorption tower cooler 12 to be condensed and enters a liquid chlorine storage tank 13, is extracted from the tower kettle, sequentially passes through the material heat exchanger 3, a primary cooler 4, a secondary cooler 5 and a tertiary cooler 6 to be cooled to 80 ℃, 40 ℃, 15 ℃ and minus 10 ℃, continuously enters the absorption tower 1, one part enters the packing layer at a flow rate of 23T/h, and the other part enters the bubble cap at a flow rate of 1T/h.And (3) a layer. The volume fractions of the absorbed tail gas components air/hydrogen/chlorine are shown in table 1, and the tail gas enters the tail gas alkaline washing tower 18 to remove chlorine and then enters the incineration device 82 for incineration. Chlorine recovery is shown in table 2.
Example 6
A method for recovering chlorine gas from tail chlorine, comprising the steps of:
the process was carried out using the apparatus of example 1 and the gas-to-liquid flow ratio of example 4, with tail chlorine having the composition of 70% chlorine, 29.8% air, 0.2% hydrogen at a flow rate of 500Nm from a chlor-alkali plant3h enters the bottom of an absorption tower 1, is sprayed with carbon tetrachloride with the temperature of minus 5 ℃ and the flow rate of 24T/h for contact mass transfer with the absorption tower 1, the chlorine in the tail chlorine flows out of the tower kettle together with the carbon tetrachloride after being absorbed, passes through a material heat exchanger 3, the temperature is raised to 60 ℃, then enters the middle part of a desorption tower 10, the chlorine is heated and is separated from the carbon tetrachloride, the pressure of the desorption tower is controlled to be 0.3MPa (P), the kettle temperature is 128 ℃, the chlorine is desorbed from the top of the tower, is condensed by a desorption tower cooler 12 and enters a liquid chlorine storage tank 13, the carbon tetrachloride is extracted from the tower kettle, and is cooled to 80 ℃, 40 ℃, 15 ℃ and minus 10 ℃ by the material heat exchanger 3, a primary cooler 4, a secondary cooler 5 and a tertiary cooler 6 in sequence, continuing to the absorption column 1, one part enters the packing layer at a flow rate of 23T/h, and the other part enters the bubble cap layer at a flow rate of 1T/h. The volume fractions of the absorbed tail gas components air/hydrogen/chlorine are shown in table 1, the tail gas enters a tail gas alkaline washing tower 81 to remove chlorine and then enters an incineration device 82 for incineration, and the chlorine recovery rate is shown in table 2.
TABLE 2 recovery of chlorine in tail chlorine/% under different conditions
As can be seen from Table 2, the highest chlorine recovery was obtained from the tail chlorine recovered by the apparatus of example 1 and the process of example 4, i.e., when the absorption column was bubble-capA packing combined tower, carbon tetrachloride as solvent and 125:6Nm of volume flow rate of tail chlorine and mass flow rate of solvent3At a desorption temperature of 130 ℃, the chlorine recovery rate reaches the highest and is 99.9 percent.
Claims (10)
1. The method for recovering chlorine in tail chlorine is characterized by comprising the following steps of solvent absorption, solvent desorption, liquid chlorine storage and tail gas treatment:
solvent absorption: tail chlorine from a chlor-alkali plant enters the lower part of the absorption tower, and the solvent is sprayed from the upper part of the absorption tower, wherein the flow rate of the tail chlorine is 500-600Nm3The flow rate of the solvent is 20-24T/h;
and (3) solvent desorption: discharging the chlorine absorbing solvent from the bottom of the absorption tower, preheating the chlorine absorbing solvent, desorbing the chlorine absorbing solvent in a desorption tower, cooling the desorbed solvent, refluxing the cooled solvent in the absorption tower for cyclic utilization, and storing the desorbed chlorine;
liquid chlorine storage: condensing the chlorine obtained by desorption, and storing the chlorine in a liquid chlorine storage tank;
tail gas treatment: tail chlorine which is not absorbed by the solvent is discharged after condensation, alkali liquor absorption and incineration in sequence.
2. The method of claim 1, wherein the tail chlorine comprises, in volume fraction: chlorine gas 60-80%, air 20-40%, and trace hydrogen; further preferably, the tail chlorine comprises, in volume fraction: 70% of chlorine, 29.8% of air and 0.2% of hydrogen.
3. The method for recovering chlorine from tail chlorine as claimed in claim 2, wherein the solvent is a chloride such as dichloromethane, trichloromethane, carbon tetrachloride and tetrachloroethylene, and more preferably, the solvent is carbon tetrachloride.
4. The method for recovering chlorine from tail chlorine as claimed in claim 3, wherein the solvent absorption temperature is-15 to 0 ℃ and the pressure is 0 to 0.05MPa (P), and more preferably the pressure is 0 to 0.02MPa (P).
5. The method for recovering chlorine in tail chlorine as claimed in claim 4, wherein the ratio of the volume flow rate of the tail chlorine absorbed by the solvent to the mass flow rate of the solvent is 125 (5-6) Nm3/T。
6. The method for recovering chlorine in tail chlorine as claimed in claim 5, wherein the desorption pressure is 0.3-0.4MPa (P), the temperature at the top of the desorption tower is 0-10 ℃, and the temperature at the bottom of the desorption tower is 125-135 ℃; preferably, the temperature of the top of the desorption tower is 0-5 ℃, and the temperature of the bottom of the desorption tower is 128-132 ℃.
7. The device adopted by the method according to claim 1, which comprises an absorption circulation unit, a desorption unit, a storage unit and a tail gas treatment unit, wherein one end of the absorption circulation unit is sequentially connected with the desorption unit and the storage unit, and the other end of the absorption circulation unit is connected with the tail gas treatment unit;
the absorption circulation unit comprises an absorption tower, a carbon tetrachloride circulation pump, a material heat exchanger, a cooler and an absorption tower condenser, wherein a foam cover layer positioned on the upper layer and a packing layer positioned on the lower layer are arranged in the absorption tower; the tower bottom of the absorption tower is connected with a low-temperature inlet of a material heat exchanger through a carbon tetrachloride circulating pump, a low-temperature outlet of the material heat exchanger is connected with a first-stage cooler, a high-temperature outlet is connected with a high-temperature inlet and a desorption unit, the third-stage cooler is respectively connected with an upper reflux inlet and a middle reflux inlet of the absorption tower, the upper reflux inlet is arranged above the bubble cap layer, and the middle reflux inlet is arranged above the packing layer and below the bubble cap layer;
the desorption unit comprises a desorption tower, a desorption tower material pump and a desorption tower reboiler; the high-temperature outlet of the material heat exchanger is connected with the middle part of the desorption tower, the bottom of the desorption tower is connected with the high-temperature inlet of the material heat exchanger through a desorption tower material pump, the bottom of the desorption tower is connected with a desorption tower reboiler, and the top of the desorption tower is connected with a storage unit;
the storage unit comprises a desorption tower cooler and a liquid chlorine storage tank, wherein the desorption tower cooler is a carbon steel tubular heat exchanger; the top of the desorption tower is connected with a liquid chlorine storage tank through a desorption tower cooler;
the tail gas treatment unit comprises a tail gas alkaline washing tower and an incineration device; one end of the tail gas alkaline washing tower is connected with the top of the absorption tower through an absorption tower condenser, and the other end of the tail gas alkaline washing tower is connected with an incineration device;
the devices are connected through pipelines.
8. The device according to claim 7, wherein the blister layer comprises 5-7 layers of blisters, preferably 6 layers of blisters, the filler layer comprises 6-12 meters of filler, preferably 8 meters of filler, and the filler is stainless steel mesh filler CY 700.
9. The apparatus of claim 8, wherein the desorber is a packed tower and the packing of the desorber is stainless steel mesh packing CY 700.
10. The device of claim 9, wherein the operating pressure of the liquid chlorine storage tank is 0.3-0.4mpa (p), and the tail gas absorption tower contains an alkali solution, wherein the alkali solution is a 10% NaOH solution by mass fraction.
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| CN114159934A (en) * | 2021-11-12 | 2022-03-11 | 浙江省天正设计工程有限公司 | Recovery device and treatment process for chlorothalonil chlorinated tail gas |
| CN114191948A (en) * | 2021-12-21 | 2022-03-18 | 湖北葛化华祥化学有限公司 | Device and method for drying chlorine gas by bubble cap drying tower |
| CN115957597A (en) * | 2022-11-25 | 2023-04-14 | 新疆敦华绿碳技术股份有限公司 | Desorption device and carbon dioxide production system |
| CN118217770A (en) * | 2024-05-08 | 2024-06-21 | 西安交通大学 | Comprehensive treatment system and process for waste salt and white carbon black tail gas in organosilicon industry |
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