CN106914097B - Recovering SO-containing material 2 Device and method for HCl tail gas - Google Patents
Recovering SO-containing material 2 Device and method for HCl tail gas Download PDFInfo
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- CN106914097B CN106914097B CN201710161946.XA CN201710161946A CN106914097B CN 106914097 B CN106914097 B CN 106914097B CN 201710161946 A CN201710161946 A CN 201710161946A CN 106914097 B CN106914097 B CN 106914097B
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 9
- 238000010521 absorption reaction Methods 0.000 claims abstract description 97
- 238000001179 sorption measurement Methods 0.000 claims abstract description 76
- 239000002808 molecular sieve Substances 0.000 claims abstract description 73
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000007788 liquid Substances 0.000 claims abstract description 47
- 230000002745 absorbent Effects 0.000 claims abstract description 27
- 239000002250 absorbent Substances 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 24
- 239000012047 saturated solution Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000007791 liquid phase Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000007792 gaseous phase Substances 0.000 claims description 2
- 230000003139 buffering effect Effects 0.000 claims 1
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 87
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 85
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- 150000001298 alcohols Chemical group 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
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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
- B01D53/1456—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
- B01D53/005—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 heat treatment
-
- 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
- B01D53/02—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 adsorption, e.g. preparative gas chromatography
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
-
- 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
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
-
- 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
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0718—Purification ; Separation of hydrogen chloride by adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
- B01D2252/103—Water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/80—Water
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Treating Waste Gases (AREA)
Abstract
Recovering SO-containing material 2 The device comprises a gas-liquid filter, an absorption device, a molecular sieve adsorption tower and an HCl rectifying tower which are connected in sequence according to the treatment sequence; in addition, the treatment step of the method is absorption-adsorption-rectification. The invention has high tail gas purifying rate, HCl and SO 2 The recovery rate of the catalyst is high, the absorbent can be recycled, the environmental pollution caused by emission is avoided, the production cost is reduced, and the economic benefit is improved.
Description
Technical Field
The invention relates to a method for recycling SO-containing components 2 An HCl tail gas device and method belong to the technical field of substance separation in chemical industry.
Background
Containing SO 2 The mixed gas with HCl is common in the production process of pharmaceutical intermediates, such as the decomposition reaction of thionyl chloride, which generates a large amount of SO 2 And HCl gas, which has strong irritation and corrosion, needs to be recycled, otherwise causes great harm to the environment.
At present, the absorption method and the freezing method are used in the common industrial methods at home and abroad. The absorption method adopts water to absorb HCl in the mixed gas, but due to SO 2 The hydrochloric acid formed by absorbing HCl by water often contains about 1% by mass of SO because of a certain solubility in water 2 The irritation is great, and the subsequent comprehensive utilization can not be performed. The freezing method utilizes SO at low temperature 2 Easy coolingThe mixed gas is separated after being cooled due to the coagulation characteristic, but SO 2 The condensation temperature is lower than-10 ℃, and additional refrigeration is needed for separation; meanwhile, the single condensation separation effect is not ideal, multi-stage separation is needed, and the equipment investment and the operation cost are relatively high.
Disclosure of Invention
The invention provides a method for recycling SO-containing materials, which aims at overcoming the defects existing in the prior art 2 Apparatus and method for HCl tail gas.
One technical proposal for solving the technical problems is as follows, one of the invention is to recycle the SO-containing liquid 2 The device of HCl tail gas, the device is according to the treatment order including the connection in proper order:
a gas-liquid filter;
the absorption device comprises an absorption tower, and the bottom of the absorption tower is communicated with the top outlet of the gas-liquid filter;
the molecular sieve adsorption tower is characterized in that a feed inlet of the molecular sieve adsorption tower is communicated with the tower kettle of the absorption tower;
the HCl rectifying tower is communicated with a discharge port of the molecular sieve adsorption tower;
SO 2 the rectifying tower, SO2 rectifying tower is communicated with the tower kettle of the HCl rectifying tower, SO 2 The tower bottom of the rectifying tower is connected with an absorbent buffer tank.
In conclusion, the device takes a gas-liquid filter as the initial end of tail gas treatment, takes absorption tower and molecular sieve adsorption as the intermediate process, and takes an HCl rectifying tower and SO 2 The rectifying tower is used as a terminal to form a complete process of the tail gas treatment device.
Further, the absorption tower is at least one stage; when the multistage absorption towers are arranged, the molecular sieve absorption towers are communicated with the first-stage absorption tower, the multistage absorption towers are connected in series, the top of the former-stage absorption tower is communicated with the bottom of the latter-stage absorption tower, the adjacent absorption towers are communicated by a circulating pipeline, and the absorbent buffer tank is connected with the last-stage absorption tower by the pipeline.
Further, a circulating pump and a cooler are arranged on a pipeline between the top of each absorption tower and the tower kettle; the tower kettle of the HCl rectifying tower is connected with a HCl reboiler, and the top of the HCl rectifying tower is provided with a HCl tower top condenserAn HCl product buffer tank is arranged below the HCl tower top condenser, and the output end of the HCl product buffer tank is connected with the HCl rectifying tower top; the SO 2 The tower kettle of the rectifying tower is connected with SO 2 Reboiler, SO 2 SO is arranged at the top of the rectifying tower 2 Overhead condenser, SO 2 SO is arranged under the tower top condenser 2 Product buffer tank, SO 2 The output end of the product buffer tank is connected with SO 2 The top of the rectifying tower.
Further, a solution tank is arranged on a pipeline between the HCl rectifying tower and a discharge port of the molecular sieve adsorption tower; the gas-liquid filter is provided with a feed inlet, the top of the gas-liquid filter is provided with a gas outlet, and the lower part of the gas-liquid filter is provided with a condensate outlet; the top of the last-stage absorption tower is provided with a non-condensable gas outlet; the molecular sieve adsorption towers are provided with high-pressure nitrogen inlets, the number of the molecular sieve adsorption towers is not less than one, and a plurality of molecular sieve adsorption towers are arranged in parallel and can be used simultaneously or alternately.
Further, the HCl product buffer tank is connected with an adsorption drying system.
Further, the SO 2 The product buffer tank is connected with an adsorption drying system.
Another technical proposal for solving the technical problems is as follows, a method for recycling SO-containing 2 A process for HCl off-gas comprising the steps of:
(1) Absorption of
Tail gas enters from the tower bottom of the first-stage absorption tower, is absorbed by the first-stage absorption tower, and the saturated solution is conveyed to the molecular sieve absorption tower;
(2) Adsorption of
Removing water from the saturated solution through a molecular sieve adsorption tower, discharging the saturated solution from the molecular sieve adsorption tower, and feeding the saturated solution into an HCl rectifying tower;
(3) Rectifying
The HCl rectifying tower is pressurized, saturated solution entering the HCl rectifying tower is subjected to heat and mass transfer process, gaseous phase HCl rising to the tower top is condensed to obtain liquid phase HCl product, and solution at the tower bottom of the HCl rectifying tower is conveyed to SO 2 In the rectifying tower;
SO 2 the rectifying tower is pressurized and enters SO 2 Saturated solution in the rectifying tower rises to gas phase SO at the top of the tower through heat and mass transfer process 2 Condensing to obtain liquid phase SO 2 Product, at SO 2 And obtaining a solution containing the absorbent at the bottom of the rectifying tower.
Further, the tail gas is filtered and separated before entering the first-stage absorption tower: introducing the tail gas into a gas-liquid filter, discharging condensate from the lower part of the gas-liquid filter, and containing HCl and SO 2 The secondary tail gas of the gas-liquid filter is discharged from the upper part of the gas-liquid filter and enters from the tower bottom of the first-stage absorption tower.
Further, in the step (1), the unabsorbed tail gas discharged from the top of the first stage absorber enters the next stage absorber and finally enters the last stage absorber; a circulating pump and a cooler are arranged on the pipeline between the top of each absorption tower and the tower kettle, and for each absorption tower, the solution circulates between the inside of each absorption tower and the cooler through the circulating pump, and in the step (3), SO is contained in the solution 2 And returning the solution containing the absorbent obtained from the tower bottom of the rectifying tower to the last stage of the absorbing tower for recycling.
Further, an HCl reboiler is connected to the tower bottom of the HCl rectifying tower, an HCl tower top condenser is arranged at the top of the HCl rectifying tower, an HCl product buffer tank is arranged below the HCl tower top condenser, the HCl product buffer tank is connected with an adsorption drying system, and the output end of the HCl product buffer tank is connected with the top of the HCl rectifying tower; the SO 2 The tower kettle of the rectifying tower is connected with SO 2 Reboiler of SO 2 SO is arranged at the top of the rectifying tower 2 Overhead condenser, SO 2 SO is arranged under the tower top condenser 2 Product buffer tank, SO 2 The product buffer tank is connected with an adsorption drying system and SO 2 The output end of the product buffer tank is connected with SO 2 The top of the rectifying tower.
Further, a solution tank is arranged on a pipeline between the HCl rectifying tower and a discharge port of the molecular sieve adsorption tower; the gas-liquid filter is provided with a feed inlet, the top of the gas-liquid filter is provided with a gas outlet, and the lower part of the gas-liquid filter is provided with a condensate outlet; the top of the last-stage absorption tower is provided with a non-condensable gas outlet; the molecular sieve adsorption towers are provided with high-pressure nitrogen inlets, the number of the molecular sieve adsorption towers is not less than one, and a plurality of molecular sieve adsorption towers are arranged in parallel and can be used simultaneously or alternately.
Further, the absorbent in the absorption tower is an organic solvent, and the absorbent is selected from alcohols, ketones, esters, ethers and other organic solvents, wherein the alcohols comprise methanol, ethanol, isopropanol, butanol and the like, the ketones comprise acetone, butanone, 2-pentanone and the like, and the esters comprise ethyl formate, methyl acetate and the like.
The process method and the device have the beneficial effects that: (1) The absorbent absorbs HCl and SO containing 2 Is an exothermic process, and HCl and SO are discharged from the absorption tower at too high temperature 2 The secondary tail gas of the gas turbine is increased, the absorption effect is reduced, a cooler is additionally arranged behind a circulating pump, the temperature of the solution is reduced, and the low-temperature solution directly contacts with the high-temperature solution to achieve the purpose of reducing the temperature in an absorption tower; (2) The absorbent can be reused, so that the environmental pollution caused by emission is avoided, the production cost is reduced, and the economic benefit is improved; (3) HCl and SO 2 Is completely separated from HCl and SO 2 The recovery rate of the catalyst is high and can reach more than 99.9 percent; (4) The molecular sieve adsorption tower can be recycled, so that the cost is saved, and the efficiency is improved; (5) The invention has high practical value and great market demand.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an embodiment of the present invention.
Wherein, the gas-liquid filter 1; a first-stage absorption column 2; a second-stage absorption column 3; a molecular sieve adsorption tower 4; a No. 1 molecular sieve adsorption tower 4-1; a No. 2 molecular sieve adsorption tower 4-2; a solution tank 5; HCl rectifying column 6; SO (SO) 2 A rectifying column 7; a circulation pump 8; a cooler 9; HCl reboiler 10; an HCl column top condenser 11; HCl product buffer tank 12; SO (SO) 2 A reboiler 13; SO (SO) 2 An overhead condenser 14; SO (SO) 2 A product buffer tank 15; an absorbent surge tank 16; and an adsorption drying system 17.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
As shown in FIG. 1, a recovered SO-containing 2 The device for the HCl tail gas comprises a gas-liquid filter 1, an absorption device, a molecular sieve adsorption tower 4, an HCl rectifying tower 6 and SO 2 Rectifying column 7, wherein:
the gas-liquid filter 1 is used for filtering water and condensate in the tail gas, a feed inlet is arranged on the gas-liquid filter 1, a gas outlet is arranged at the top of the gas-liquid filter, and a condensate outlet is arranged at the lower part of the gas-liquid filter;
the absorption device comprises two stages of absorption towers, the number of which is a first stage absorption tower 2 and a second stage absorption tower 3, the tower bottom of the first stage absorption tower 2 is communicated with the top outlet of the gas-liquid filter 1, the tower top of the first stage absorption tower 2 is communicated with the tower bottom of the second stage absorption tower 3, the two-way conveying of materials can realize the internal circulation of the first stage absorption tower 2 and the second stage absorption tower 3, and the tower top of the second stage absorption tower 3 is provided with a noncondensable gas outlet; the circulating pump 8 and the cooler 9 are arranged on the pipelines between the tower top and the tower bottom of the first-stage absorption tower 2 and between the tower top and the tower bottom of the second-stage absorption tower 3, and the tower bottom of the first-stage absorption tower 2 is communicated with the tower bottom feed inlet of the molecular sieve absorption tower 4; the material circulation between the first-stage absorption tower 2 and the second-stage absorption tower 3 and the material transportation are realized by arranging a remote transmission liquid level meter linkage regulating valve, a flow meter linkage regulating valve or a remote transmission liquid level meter and a flow meter linkage regulating valve on a circuit.
The molecular sieve adsorption towers 4, the molecular sieve adsorption towers 4 are provided with high-pressure nitrogen inlets, the number of the molecular sieve adsorption towers 4 is two, the number of the No. 1 molecular sieve adsorption towers 4-1 and the number of the No. 2 molecular sieve adsorption towers 4-2, the two molecular sieve adsorption towers 4 are arranged in parallel between the tower kettle of the first-stage absorption tower 2 and the HCl rectifying tower 6, and the two molecular sieve adsorption towers 4 can be used simultaneously or alternatively;
the middle part of the HCl rectifying tower 6 is communicated with the top discharge ports of the No. 1 molecular sieve adsorption tower 4-1 and the No. 2 molecular sieve adsorption tower 4-2, and a solution tank 5 is arranged on a pipeline between the top discharge ports of the HCl rectifying tower 6 and the No. 1 molecular sieve adsorption tower 4-1 and the No. 2 molecular sieve adsorption tower 4-2; the tower bottom of the HCl rectifying tower 6 is connected with a HCl reboiler 10, a HCl tower top condenser 11 is arranged at the tower top of the HCl rectifying tower 6, a HCl product buffer tank 12 is arranged below the HCl tower top condenser 11, the HCl product buffer tank 12 is connected with an adsorption drying system 17, and the output end of the HCl product buffer tank 12 is connected with the tower top of the HCl rectifying tower 6;
SO 2 rectifying column 7, SO 2 The middle part of the rectifying tower 7 is communicated with the tower kettle of the HCl rectifying tower 6, SO 2 The tower bottom of the rectifying tower 7 is connected with an absorbent buffer tank 16; SO (SO) 2 The tower kettle of the rectifying tower 7 is connected with SO 2 Reboiler 13, SO 2 SO is arranged at the top of the rectifying tower 7 2 Overhead condenser 14, SO 2 SO is arranged under the tower top condenser 14 2 Product buffer tank 15, SO 2 The product buffer tank 15 is connected with an adsorption drying system 17 and SO (SO) 2 The output end of the product buffer tank 15 is connected with SO 2 The top of the rectifying tower 7.
The absorbent buffer tank 16 is also connected with the second-stage absorption tower 3 through a pipeline, and a remote transmission liquid level meter linkage adjusting valve, a flowmeter linkage adjusting valve or a remote transmission liquid level meter and a flowmeter linkage adjusting valve are arranged on the pipeline, SO that the absorbent in the absorbent buffer tank 16 is automatically input into the second-stage absorption tower 3, and the second-stage absorption tower 3 and SO 2 The return circulation of the absorbent is completed between the rectifying towers 7.
The device takes a gas-liquid filter 1 as the initial end of tail gas treatment, takes absorption tower and molecular sieve adsorption as the intermediate process, and takes an HCl rectifying tower 6 and SO 2 The rectifying tower 7 is a terminal, and forms a complete process of tail gas treatment.
Example 2
Referring to fig. 2, in example 1, the number of molecular sieve adsorption columns 4 is one, the bottoms of the molecular sieve adsorption columns 4 are discharge ports, the tops of the columns are feed ports, and the number of the adsorption columns is one.
Example 3
(1) Absorption of
Tail gas enters from the tower kettle of the first-stage absorption tower 2, and the first-stage absorption tower 2 absorbs HCl and SO in the tail gas 2 Then, the saturated solution is conveyed to a molecular sieve adsorption tower 4, the tail gas which is not absorbed is discharged from the top of a first-stage absorption tower 2 and enters from the tower bottom of a second-stage absorption tower 3, and the unsaturated solution is obtained after being absorbed again by the second-stage absorption tower 3 and returns to the first-stage absorption tower 2; between the tower top and the tower bottom of the first-stage absorption tower 2,A circulating pump 8 and a cooler 9 are arranged on the pipeline between the tower top and the tower bottom of the second-stage absorption tower 3, and for each absorption tower, the solution circulates between the inside of each absorption tower and the cooler 9 through the circulating pump 8;
(2) Adsorption of
The saturated solution delivered from step (2) will contain a small amount of moisture, and the purpose of the adsorption section is to remove the moisture from the saturated solution. The method is specifically characterized in that saturated solution enters a molecular sieve adsorption tower 4, molecular sieves with pore channels of specific sizes are arranged in the molecular sieve adsorption tower 4, molecular sieve filling hand holes are formed in the upper portion of the molecular sieve adsorption tower 4, and a molecular sieve discharge opening is formed in the lower portion of the molecular sieve adsorption tower 4, so that the molecular sieves can be conveniently replaced. The saturated solution can be passed through the molecular sieve with specific pore canal to remove the water in the saturated solution so as to attain the goal of dewatering. Meanwhile, a high-pressure nitrogen inlet is formed in the molecular sieve adsorption tower 4, the molecular sieve full of water can be purged through high-pressure nitrogen, adsorbed water is removed, online regeneration of the molecular sieve is realized, recycling is realized, cost is saved, and efficiency is improved. The water purged by the nitrogen can be discharged up to the standard or stored and reused in the corresponding working section. The saturated solution which is dehydrated is discharged from the top of a No. 1 molecular sieve adsorption tower 4-1 and a No. 2 molecular sieve adsorption tower 4-2, and enters a solution tank 5 for storage, wherein the No. 1 molecular sieve adsorption tower 4-1 and the No. 2 molecular sieve adsorption tower 4-2 can be used simultaneously or alternatively, and the No. 1 molecular sieve adsorption towers 4-1 and the No. 2 molecular sieve adsorption towers 4-2 designed by the device are alternatively used, so that the continuous and stable operation of the whole set of device is ensured when the online regeneration of molecular sieves is carried out;
(3) Rectifying
Including HCl rectification and SO 2 And (5) rectifying. The concrete operation is that the solution tank 5 contains HCl and SO 2 Is fed to HCl rectifying column 6. The HCl rectifying tower 6 is pressurized, saturated solution in the HCl rectifying tower 6 is heated by an HCl reboiler 10 and then becomes steam to rise into the HCl rectifying tower 6, the HCl rectifying tower 6 is filled with fillers, reflux liquid and rising steam are contacted with each other on each layer of filler, a heat and mass transfer process is carried out, HCl with low boiling point and easy volatilization is converted into gas phase to rise to the top of the tower, the gas phase HCl is converted into liquid phase to obtain qualified HCl products through condensation of an HCl tower top condenser 11, and the non-cold HCl products are obtainedThe small amount of non-condensable gas can be safely emptied. An HCl product buffer tank 12 is arranged at the top of the column, and part of HCl product is delivered to the HCl rectifying column 6 to maintain the balance of the HCl rectifying column 6. High boiling SO 2 And the absorbent is cooled by the refluxed liquid phase HCl and returns to the tower kettle under condensation for continuous circulation. Conveying the solution at the tower bottom of the HCl rectifying tower 6 to SO 2 A rectifying tower 7;
SO 2 the rectification column 7 is likewise operated under pressure, SO 2 Saturated solution in rectifying tower 7 is subjected to SO 2 The reboiler 13 is heated to become steam and rise to SO 2 In the rectifying column 7, SO 2 The rectifying tower 7 is filled with packing, and reflux liquid and rising steam are contacted with each other on each layer of packing to carry out heat and mass transfer process, SO that the SO with low boiling point and easy volatilization 2 Is converted into gas phase and rises to the top of the tower to pass through SO 2 Condensation of overhead condenser 14, vapor phase SO 2 Conversion to liquid phase yields acceptable SO 2 The product can be safely emptied without condensing a small amount of noncondensable gases. SO is arranged at the top of the tower 2 Product surge tank 15, part of SO 2 Delivery of product to SO 2 In the rectifying column 7 to hold SO 2 Balance of the rectifying column 7. Liquid phase SO with high boiling point absorbent being refluxed 2 Is condensed and returns to the tower kettle for continuous circulation. SO (SO) 2 The absorbent at the bottom of the rectifying tower 7 is cooled and conveyed to an absorbent buffer tank 16. The absorbent transferred to the absorbent buffer tank 16 can be recycled as fresh absorbent into the second-stage absorption tower 3.
Example 4
On the basis of the embodiment 3, the filtering and separating operation is added before the step (1), so that the gas and liquid can be separated more effectively firstly: will contain SO 2 Adding the tail gas of HCl, CO, CO, water and other non-condensable gases into a gas-liquid filter 1 containing a wire mesh demister, discharging condensate from the lower part of the gas-liquid filter 1 to a corresponding working section for storage or direct discharge, and containing HCl and SO 2 The secondary tail gas of the gas-liquid filter 1 is discharged from the upper part of the gas-liquid filter and enters from the tower bottom of the first-stage absorption tower 2.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (8)
1. Recovering SO-containing material 2 The device of HCl tail gas, its characterized in that, the device includes the connection according to the processing sequence in proper order:
the tail gas is introduced into the gas-liquid filter, and the condensate is discharged from the lower part of the gas-liquid filter and contains HCl and SO 2 The secondary tail gas of the gas-liquid filter is discharged from the upper part of the gas-liquid filter and enters from the tower bottom of the first-stage absorption tower;
the absorption device comprises an absorption tower, the bottom of the absorption tower is communicated with the top outlet of the gas-liquid filter, and the absorbent in the absorption tower is an organic solvent;
the molecular sieve adsorption tower, the molecular sieve adsorption tower feed inlet is communicated with the tower kettle of the adsorption tower, and the saturated solution can remove the moisture in the saturated solution through the molecular sieve of the specific pore canal so as to achieve the purpose of dehydration;
the HCl rectifying tower is communicated with a discharge port of the molecular sieve adsorption tower;
SO 2 rectifying tower, SO 2 The rectifying tower is communicated with the tower kettle of the HCl rectifying tower, SO 2 The tower bottom of the rectifying tower is connected with an absorbent buffer tank;
the absorption tower is at least one stage; when the multistage absorption towers are arranged, the molecular sieve absorption towers are communicated with the first-stage absorption tower, the multistage absorption towers are connected in series, the top of the former-stage absorption tower is communicated with the bottom of the latter-stage absorption tower, the adjacent absorption towers are communicated by a circulating pipeline, and the absorbent buffer tank is connected with the last-stage absorption tower by the pipeline.
2. A recovered SO-containing product according to claim 1 2 The device for the HCl tail gas is characterized in that a circulating pump and a cooler are arranged on a pipeline between the top of each absorption tower and the tower kettle; the HCl rectifying tower kettle is connected with a HCl reboiler, the HCl rectifying tower top is provided with a HCl tower top condenser, a HCl product buffer tank is arranged below the HCl tower top condenser, and the HCl product buffer tank is connected with an adsorption drying system, and is used for buffering HCl productsThe output end of the tank is connected with the top of the HCl rectifying tower; the SO 2 The tower kettle of the rectifying tower is connected with SO 2 Reboiler, SO 2 SO is arranged at the top of the rectifying tower 2 Overhead condenser, SO 2 SO is arranged under the tower top condenser 2 Product buffer tank, SO 2 The product buffer tank is connected with an adsorption drying system and SO 2 The output end of the product buffer tank is connected with SO 2 The top of the rectifying tower.
3. A recovered SO-containing product according to claim 1 2 The device for the HCl tail gas is characterized in that a solution tank is arranged on a pipeline between the HCl rectifying tower and a discharge port of the molecular sieve adsorption tower; the gas-liquid filter is provided with a feed inlet, the top of the gas-liquid filter is provided with a gas outlet, and the lower part of the gas-liquid filter is provided with a condensate outlet; the molecular sieve adsorption towers are provided with high-pressure nitrogen inlets, the number of the molecular sieve adsorption towers is not less than one, and a plurality of molecular sieve adsorption towers are arranged in parallel and can be used simultaneously or alternately.
4. Recovering SO-containing material 2 A process for recovering SO-containing tail gas by using the method as claimed in any one of claims 1 to 3 2 The device for the HCl tail gas is characterized by comprising the following steps of:
(1) Absorption of
Tail gas enters from the tower bottom of the first-stage absorption tower, is absorbed by the first-stage absorption tower, and the saturated solution is conveyed to the molecular sieve absorption tower;
(2) Adsorption of
Removing water from the saturated solution through a molecular sieve adsorption tower, discharging the saturated solution from the molecular sieve adsorption tower, and feeding the saturated solution into an HCl rectifying tower;
(3) Rectifying
The HCl rectifying tower is pressurized, saturated solution entering the HCl rectifying tower is subjected to heat and mass transfer process, gaseous phase HCl rising to the tower top is condensed to obtain liquid phase HCl product, and solution at the tower bottom of the HCl rectifying tower is conveyed to SO 2 In the rectifying tower;
SO 2 the rectifying tower is pressurized and enters SO 2 Saturated solution in rectifying tower is transferred by heat and massThe process, gas phase SO rising to the top of the column 2 Condensing to obtain liquid phase SO 2 Product, at SO 2 And obtaining a solution containing the absorbent at the bottom of the rectifying tower.
5. A recovered SO-containing product according to claim 4 2 The method for preparing the HCl tail gas is characterized in that the tail gas is filtered and separated before entering a first-stage absorption tower: introducing the tail gas into a gas-liquid filter, discharging condensate from the lower part of the gas-liquid filter, and containing HCl and SO 2 The secondary tail gas of the gas-liquid filter is discharged from the upper part of the gas-liquid filter and enters from the tower bottom of the first-stage absorption tower.
6. A recovered SO-containing product according to claim 4 2 The method for preparing HCl tail gas is characterized in that in the step (1), the unabsorbed tail gas discharged from the top of a first-stage absorption tower enters a next-stage absorption tower and finally enters a last-stage absorption tower; a circulating pump and a cooler are arranged on the pipeline between the top of each absorption tower and the tower kettle, and for each absorption tower, the solution circulates between the inside of each absorption tower and the cooler through the circulating pump, and in the step (3), SO is contained in the solution 2 And returning the solution containing the absorbent obtained from the tower bottom of the rectifying tower to the last stage of the absorbing tower for recycling.
7. A recovered SO-containing product according to claim 4 2 The method for preparing the HCl tail gas is characterized in that an HCl reboiler is connected to the tower bottom of the HCl rectifying tower, an HCl tower top condenser is arranged at the top of the HCl rectifying tower, an HCl product buffer tank is arranged below the HCl tower top condenser, the HCl product buffer tank is connected with an adsorption drying system, and the output end of the HCl product buffer tank is connected with the top of the HCl rectifying tower; the SO 2 The tower kettle of the rectifying tower is connected with SO 2 Reboiler of SO 2 SO is arranged at the top of the rectifying tower 2 Overhead condenser, SO 2 SO is arranged under the tower top condenser 2 Product buffer tank, SO 2 The product buffer tank is connected with an adsorption drying system and SO 2 The output end of the product buffer tank is connected with SO 2 The top of the rectifying tower.
8. A recovered SO-containing product according to claim 4 2 The method for preparing the HCl tail gas is characterized in that a solution tank is arranged on a pipeline between a HCl rectifying tower and a discharge port of a molecular sieve adsorption tower; the gas-liquid filter is provided with a feed inlet, the top is provided with a gas outlet, and the lower part is provided with a condensate outlet; the molecular sieve adsorption towers are provided with high-pressure nitrogen inlets, the number of the molecular sieve adsorption towers is not less than one, and a plurality of molecular sieve adsorption towers are arranged in parallel and can be used simultaneously or alternately.
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| CN107774097A (en) * | 2017-09-29 | 2018-03-09 | 北京石油化工学院 | A kind of handling process of VOCs waste gas |
| CN107803098A (en) * | 2017-09-29 | 2018-03-16 | 北京石油化工学院 | A kind of handling process of VOCs waste gas |
| CN118179218A (en) * | 2024-04-02 | 2024-06-14 | 江苏维尤纳特精细化工有限公司 | Treatment method and treatment equipment for tail gas in chlorination production |
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