CN110655042A - Method and device for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur - Google Patents
Method and device for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur Download PDFInfo
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- CN110655042A CN110655042A CN201910078067.XA CN201910078067A CN110655042A CN 110655042 A CN110655042 A CN 110655042A CN 201910078067 A CN201910078067 A CN 201910078067A CN 110655042 A CN110655042 A CN 110655042A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 168
- 239000011593 sulfur Substances 0.000 title claims abstract description 168
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 52
- 239000007789 gas Substances 0.000 title claims abstract description 46
- 239000002912 waste gas Substances 0.000 title claims abstract description 33
- 229920000297 Rayon Polymers 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims description 26
- 239000007788 liquid Substances 0.000 claims abstract description 178
- 238000005406 washing Methods 0.000 claims abstract description 165
- 229910001868 water Inorganic materials 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002844 melting Methods 0.000 claims abstract description 28
- 230000008018 melting Effects 0.000 claims abstract description 28
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 238000005507 spraying Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 8
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000008187 granular material Substances 0.000 claims abstract 2
- 239000006260 foam Substances 0.000 claims description 22
- 239000005864 Sulphur Substances 0.000 claims description 12
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 229960001484 edetic acid Drugs 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 7
- 239000008234 soft water Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 239000006228 supernatant Substances 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003599 detergent Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 18
- -1 sulfur ions Chemical class 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910001448 ferrous ion Inorganic materials 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 239000008188 pellet Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000002738 chelating agent Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910001447 ferric ion Inorganic materials 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- FLTRNWIFKITPIO-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe] FLTRNWIFKITPIO-UHFFFAOYSA-N 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000002894 organic compounds Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- 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
- C01B17/02—Preparation of sulfur; Purification
- C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
- C01B17/05—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by wet processes
-
- 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
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0221—Melting
-
- 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
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0232—Purification, e.g. degassing
Abstract
A process for preparing sulfur from the hydrogen sulfide gas in viscose waste gas includes such steps as preparing the washing solution from EDTA, triethanolamine, ferrous sulfate, sodium carbonate and water; washing solution pump in H2S, spraying by using a washing tower, wherein viscose waste gas enters from the bottom of the washing tower and is fully contacted with a washing solution in a countercurrent mode, and hydrogen sulfide in the viscose waste gas is absorbed by the washing solution; sending the liquid flowing out from the bottom of the washing tower to a centrifuge, wherein the liquid contains enriched elemental sulfur; sending the concentrated sulfur slurry separated by the centrifuge to a sulfur recovery device; heating the sulfur in a sulfur recovery device to 135 ℃ and then melting the sulfur into liquid sulfur, sending the pure sulfur liquid to a sulfur granulator, separating the sulfur liquid into small liquid drops, cooling the liquid drops to 50 ℃ and solidifying the liquid drops to obtain sulfur granules. The invention has the beneficial effects that: the selective treatment of hydrogen sulfide can be carried out from viscose waste gas without consuming a large amount of detergent and heating and pressurizingRecovering hydrogen sulfide gas to prepare sulfur.
Description
Technical Field
The invention belongs to the field of hydrogen sulfide treatment processes, and particularly relates to a method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur and a special device.
Background
In the prior art, for CS2And H2The treatment method of the S mixed gas comprises the following steps:
1. separately treating with alkaline absorbent (such as NaOH or Na)2CO3Or NaHCO3Aqueous solution of (b) absorb H therein2S, absorbing CS in the S by using an adsorbent (activated carbon or activated fiber)2Namely alkali washing + adsorption. The method has the following defects: the by-product sodium hydrosulfide needs to be concentrated, and a large amount of sulfur-containing wastewater and miscellaneous salts are easily generated.
2. Recovery of sulfur by claus process: by making CS in exhaust gases in a Claus incinerator2And H2Oxidation of S to SO2SO formed2With H in the intake air2S is recovered by producing sulfur according to the following reaction equation:
2H2S+SO2=2H2O+3S
the amount of catalyst used is 0.1% ~ 0.2.2% of the reaction mixture, the temperature in the reactor must be less than 650 ℃, otherwise the catalyst structure is damaged and the temperature must not exceed 480 ℃ when hydrocarbons are present in the exhaust gas.
Claus process requires CS in the exhaust gas2And H2S should be initially concentrated to a concentration greater than 7-15g/Nm, otherwise, incineration cannot supply heat to meet the reaction requirements and the temperature required for normal reaction cannot be maintained.
The treatment mode has the advantages of complex process, high cost, high energy consumption and low recovery rate.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for selectively treating hydrogen sulfide, which does not consume a large amount of detergent and does not need heating and pressurizing to recover hydrogen sulfide gas from viscose waste gas to prepare sulfur.
The invention also aims to provide a special device for the method for recovering the hydrogen sulfide gas from the viscose waste gas to prepare the sulfur.
The technical conception of the invention is as follows:
H2S + 1/2 O2 → H2O + S° （1）
this reaction takes place in a water-based solution, which is accomplished by the addition of water-soluble metal ions. Because water-soluble metal ions are easily oxidized by oxygen in air or acid gas, and a stable electrode is provided to oxidize sulfur ions into elemental sulfur, because the reaction is carried out in the water-prepared washing solution, electrons of bivalent sulfur (HS-) are easily released to form elemental sulfur in the water-prepared washing solution containing the metal ions, and the electrons are transferred to the oxygen in the regeneration process. Although there are many metal ions that can accomplish the above reaction, the present invention selects iron ions because iron ions have characteristics of low cost and non-toxicity.
The invention can be divided into two parts of reaction and regeneration, which are as follows:
reaction part:
absorption of H in Water-formulated Wash solutions2S gas:
H2s (gaseous) + H2O (liquid) ↔ H2S (liquid) + H2O (liquid) (2)
Ionization:
H2s (liquid) ↔ H+ + HS- （3）
High valence iron ion (Fe)3(+) oxidized divalent sulfur:
HS- + 2Fe3+ → 2Fe2+ + H+ + S0 （4）
general equation of reaction (equations 2, 3, 4 superimposed)
H2S (gaseous) + 2Fe3+ → 2H+ + S°+ 2Fe2+ （5）
A regeneration part:
absorption of oxygen in water-formulated wash solutions:
1/2 O2(gaseous) + H2O ↔ 1/2 O2(liquid) + H2O （6）
Ferrous ion regeneration reaction (Fe)2+)
1/2 O2(liquid) + H2O + 2Fe2+ → 2OH- + 2Fe3+ （7）
Total equation of regenerative part (equations 6, 7 superimposed)
1/2 O2(gas) + H2O + 2Fe2+ → 2OH- + 2Fe3+ （8）
The overall reaction equation (superposition of equations 5, 8) is shown in (1).
In the overall reaction, the role of the iron ions is to release the electrons generated in the absorption reaction to the regeneration reaction, and since two iron atoms are consumed for each elemental sulphur generation, at least two iron atoms are provided during the reaction. Thus, iron ions are the reactant. However, iron ions are not consumed in the overall reaction and act as a catalyst for the reaction of hydrogen sulfide and oxygen. Due to this dual function, iron ion complexes are generally defined as catalytic reactants.
In water-formulated washing solutions, ferrous ions (Fe)2+) And ferric ion (Fe)3+) Cannot exist stably, and generally, iron hydroxide or iron sulfide precipitate is easily formed through the following reaction:
Fe3+ + 3OH- → Fe(OH)3(solid) (9)
Fe2+ + S2- → FeS (solid) (10)
The technical scheme of the invention is as follows: mixing EDTA (ethylene diamine tetraacetic acid), TEA (triethanolamine), ferrous sulfate and sodium carbonate according to a certain proportion to obtain a washing solution prepared by water; the washing solution is pumped into the pump by a pump H2S washing tower for spraying and viscose waste gas from H2S enters the bottom of the washing tower and is fully contacted with the washing solution in a counter-current mode, hydrogen sulfide in the viscose waste gas is absorbed by the washing solution, and absorbed H2Fe in S gas washed solution+3Catalytic oxidation to elemental sulfur; and these Fe+3Is reduced to Fe+2Then, Fe+2Is oxidized again into Fe by the oxygen in the gas3+，Fe+2With Fe+3This forms a chelate solvent (washing solution) under the action of the chelating agent, all of which are carried out in H2S in a wash columnOf (1);
washing solution is circulated in H2S, circularly spraying in a washing tower; from H2The liquid flowing out of the bottom of the S washing column contains enriched elemental sulfur, from H2S, feeding a part of liquid flowing out of the bottom of the washing tower into a demister, and blowing air into the demister to blow off elemental sulfur foam; the foam containing the elemental sulfur is collected in a foam collecting tank and is sent to a centrifuge through a foam delivery pump (a diaphragm pump); from H2Returning the other part of the liquid from the bottom of the S washing tower to the washing liquid circulating tank, replenishing the washing solution, and pumping H2S, circularly spraying at the top of the washing tower;
sending the concentrated sulfur slurry separated by the centrifuge to a sulfur slurry collecting tank, adding soft water into the sulfur slurry collecting tank, and pumping the mixture to a sulfur recovery device; heating the sulfur in a sulfur recovery device to the temperature of 120-140 ℃, melting the sulfur into liquid sulfur, discharging light liquid at the middle upper part of the liquid sulfur in a sulfur separator from the top, discharging pure liquid sulfur from the bottom, sending the pure sulfur liquid to a sulfur granulator, separating the liquid into small liquid drops, cooling the liquid drops to the temperature below 50 ℃, and solidifying the liquid drops to form sulfur particles.
The washing solution is prepared from EDTA (ethylene diamine tetraacetic acid), TEA (triethanolamine), ferrous sulfate, sodium carbonate and water in a weight ratio of (5 ~ 20) = (1 ~ 10)% (3 ~ 12)% (10 ~ 20)% to (38 ~ 81)%.
H according to the invention2And a hollow conical nozzle is arranged at the top of the S washing tower, and washing solution is pumped into the conical nozzle through a pump to be sprayed to absorb hydrogen sulfide gas in the viscose waste gas.
H according to the invention2The S washing tower has three liquid inlets, each liquid inlet is connected with H2The conical nozzles of the washing liquid sprayers inside the S washing tower are communicated, and the washing liquid flows from the H2And (S) enabling three liquid inlets on the upper part, the middle part and the lower part of the washing tower to enter three layers of spraying washing areas in the washing tower to absorb hydrogen sulfide gas in the viscose waste gas.
The invention proceeds from H2S washing the liquid flowing out of the bottom of the tower, wherein 10 percent ~ 50 percent of the liquid enters a demister.
The content of sulfur in liquid in a washing liquid circulating tank is controlled to be 0.5 ~ 15g/l, the concentration of sulfur in liquid in a foam collecting tank 8 is controlled to be 20 ~ 100g/l, and the concentration of concentrated sulfur slurry separated by a centrifugal machine is controlled to be 200 ~ 400 g/l.
The invention adds soft water into a sulfur slurry tank, and the concentration of the sulfur-containing liquid is diluted to 50 ~ 200 g/l.
In order to prevent the generation of the above-mentioned precipitate, the present invention adopts a chelating agent, so that the iron ion can be stably kept in the proportioning solution in a wide pH value range. A chelating agent is an organic compound that encapsulates a metal ion in a claw-like structure, allowing the metal ion to form a chemical bond with two or more non-metal ions.
Compared with the prior art, the invention improves the Claus reaction, provides a continuous, simple and safe method for removing hydrogen sulfide and recovering sulfur, and has the beneficial effects that: the hydrogen sulfide is selectively treated, a large amount of washing agent is not consumed, heating and pressurizing are not needed, and the hydrogen sulfide gas can be recovered from the viscose waste gas to prepare the sulfur.
Drawings
FIG. 1 is a schematic view of the structure of an absorbent portion of the present invention;
fig. 2 is a partial structure schematic diagram of the finished product of the invention.
Detailed Description
FIG. 1 includes a washing column 1 (H)2S washing tower), a demister 2, a demisting fan 3, a washing liquid circulating tank 4, a demister 5, a washing liquid circulating pump 6, a blower 7, a foam collecting tank 8, a foam conveying pump 9, a centrifuge 10, a sulfur slurry collecting tank 11, a sulfur slurry conveying pump 12, a sulfur heater 13, a sulfur melting separator 14, a sulfur melting collecting tank 15, a gas-liquid separator 16, a waste liquid collecting tank 17, a sulfur melting standing tank 18, a sulfur melting transfer tank 19, a submerged pump 20, a granulator 21, a packing machine 22, a washing liquid blending tank 23, a flash evaporation cooler 24, a water washing circulating tank 25 and a water washing pump 26. The viscose waste gas pipeline (containing hydrogen sulfide waste gas) is connected with the lower gas inlet of the washing tower 1, and the top gas outlet of the washing tower 1 is connected with the gas inlet of the demister 2. The washing tower 1 is provided with an upper liquid inlet, a middle liquid inlet and a lower liquid inlet, and three layers are arranged in the washing tower 1The washing liquid sprayer forms a three-layer spraying washing area, each liquid inlet is communicated with a conical nozzle of the washing liquid sprayer in the washing tower, and the washing solution enters the three-layer spraying washing area in the washing tower from the upper liquid inlet, the middle liquid inlet and the lower liquid inlet of the washing tower to absorb hydrogen sulfide gas in the viscose waste gas. Three inlets of the washing tower 1 are connected with a liquid outlet of the washing liquid circulating tank 4 through a washing liquid circulating pump 6, and a liquid outlet at the bottom of the washing tower 1 is respectively connected with a liquid inlet of the washing liquid circulating tank 4 and a liquid inlet of the demister 5. The branch of the liquid inlet at the upper part of the washing tower 1 is connected with the liquid outlet of the washing liquid preparation tank 23. The air outlet on the side part of the demister 2 is connected with the demisting fan 3, and the liquid outlet on the bottom is connected with the liquid inlet of the demister 5. The bottom of the demister 5 is connected with a plurality of rows of air inlet pipes, the air inlet pipes are connected with an air blower 7, a discharge hole in the upper part of the demister 7 is connected with a feed inlet of a foam collecting tank 8, and an overflow port of the demister 5 is connected with a liquid inlet of a washing liquid circulating tank 4. The discharge port of the foam collecting tank 8 is connected with the feed port of a centrifuge 10 through a foam delivery pump 9. The discharge hole of the centrifuge 10 is connected with the feed inlet of the sulfur slurry collecting tank 11, and the separation liquid outlet of the centrifuge 10 is connected with the feed inlet of the demister 5. The water replenishing pipe orifice of the sulfur slurry collecting tank 11 is connected with a soft water pipeline, and the discharge port of the sulfur slurry collecting tank 11 is connected with the top feed inlet of a sulfur heater 13 through a sulfur slurry conveying pump 12.
In FIG. 2, the discharge port of the sulfur slurry collecting tank 11 is connected with the top feed port of the sulfur heater 13 through the sulfur slurry delivery pump 12; the heating port of the sulfur heater 13 is connected with a steam heating pipeline, and the upper liquid outlet and the lower discharge port of the sulfur heater 13 are respectively connected with the upper liquid inlet and the bottom feed inlet of the sulfur melting separator 14. The mouth of the heater of the sulfur melting separator 14 is connected with a steam pipeline, the discharge hole at the lower part is connected with a sulfur melting collecting tank 15, and the waste liquid discharge hole at the top of the sulfur melting separator 14 is connected with the feed inlet of a gas-liquid separator 16. A liquid outlet at the bottom of the gas-liquid separator 16 is connected with a waste liquid collecting tank 17, and an exhaust port at the top of the gas-liquid separator 16 is connected with an air inlet at the lower part of the flash evaporator 24. An air outlet at the top of the flash cooler 24 is connected with the atmosphere, a water inlet at the upper part of the flash cooler 24 is connected with the water washing circulating tank 25 through a water washing pump 26, a water inlet of the flash cooler 24 is connected with the internal washing sprayer, a water outlet at the bottom of the flash cooler 25 is connected with a water inlet of the water washing circulating tank 25, and a water inlet of the water washing circulating tank 25 is also connected with a filtered water pipeline. The shell of the sulfur melting collecting tank 15 is provided with a jacket, and steam is introduced into the jacket. A discharge hole at the lower part of the molten sulfur collecting tank 15 is connected with a feed hole of a molten sulfur standing tank 18. The shell of the sulfur melting standing tank 18 is provided with a rubber sleeve, a coil is arranged in an inner cavity, and steam is introduced into the sleeve and the coil. The upper discharge port of the molten sulfur standing tank 18 is connected with the feed port of the molten sulfur transfer tank 19. The shell of the sulfur melting transfer tank 19 is provided with a rubber sleeve, a coil is arranged in the inner cavity, and steam is introduced into the sleeve and the coil. The inside is provided with a submerged pump 20, and the discharge port of the submerged pump 20 is connected with a granulator 21. The discharge port of the granulator 21 is connected to a baler 22.
Firstly, preparing a washing liquid in a washing liquid circulating tank 4, wherein the concentration of each component of the washing liquid comprises EDTA 10 ~ 30g/l, Na2CO 340 ~ 60g/l, TEA 1 ~ 10g/l and FeSO 420 ~ 40g/l, starting a washing liquid circulating pump 6 to enable the washing liquid to enter the washing tower 1 from three liquid inlets of the upper part, the middle part and the lower part of the washing tower 1 and to be sprayed out from a conical nozzle of a three-layer washing liquid sprayer respectively, entering a three-layer spraying washing area, and then refluxing to the washing liquid circulating tank 4 from the bottom of the washing tower 1, connecting a branch pipe of an upper liquid inlet pipe of the washing tower 1 with a washing liquid preparation tank 23, and connecting washing preparation liquid for supplementing washing liquid lost in the subsequent reaction and separation processes, starting a demisting fan 3 to guide gas containing hydrogen sulfide to enter the washing tower 1 from the lower part of the washing tower 1, removing 98% of hydrogen sulfide in the gas after the gas passes through the three-layer spraying washing area, converting the gas into washing liquid of monomer sulfur backflow, introducing the gas into the washing liquid removed from the demisting fan 3, and then flowing into the washing liquid separated by a demister 5.
Most of the washing liquid flowing out of the liquid outlet at the bottom of the washing tower 1 flows back to the washing liquid circulating tank 4. A small portion of which is diverted to the demister 5. The sulfur content of the washing liquid is just equivalent to the newly added sulfur content in the washing liquid by adjusting the flow of the part of the shunted washing liquid, so that the stability of the sulfur content of the washing liquid circulating tank 4 can be kept, and the newly added sulfur can be transferred out.
The sulfur liquid in the demister 5 is floated on the surface of the demister by bubbles introduced into the demister, and then is scraped and flows to a foam collecting tank 8 by a spiral scraper arranged on the liquid surface of the upper part of the demister. And the redundant washing liquid in the demister 5 flows back to the washing liquid circulating tank 4 from the demister overflow port.
The foam collecting tank 8 is provided with a stirrer, and the purpose of preventing sulfur precipitation is achieved. The sulphur liquid in the foam collecting tank 8 is sent to a centrifuge 10 by a foam transfer pump 9, and the concentrated sulphur slurry separated by the centrifuge 10 is sent to a sulphur slurry collecting tank 11. The washing liquid separated by the centrifuge 10 is returned to the demister 5.
Soft water is added into a sulfur slurry collecting tank 11, the concentration of sulfur-containing liquid is diluted to 50 ~ 200g/l, the sulfur-containing liquid is evenly stirred and then is sent into a shell of a sulfur heater 13 through a sulfur slurry conveying pump 12, steam is introduced into an interlayer of the shell of the sulfur heater 13 and a heating pipe inserted into the interlayer, the sulfur-containing liquid entering the sulfur heater is heated, the sulfur is heated and melted into liquid at the temperature of 120 to 120 ~ 140 ℃, the liquid is sunk into the bottom of the sulfur heater 13 and enters the lower part of a cavity of a sulfur melting separator 14 through a discharge hole at the bottom of the sulfur heater, and light liquid at the upper part of the sulfur heater 13 enters the upper part of the cavity of the sulfur melting separator 14.
Steam is introduced into an interlayer of the shell of the sulfur melting separator 14 and a heating pipe inserted into the sulfur melting separator 14, so that the purposes of heating, heat preservation and separation of the incoming molten sulfur and light liquid are achieved, the molten sulfur separated from the bottom of the sulfur melting separator enters a sulfur melting collecting tank 15, the concentration of the sulfur in the molten sulfur reaches 95 ~ 99%, and the light liquid on the upper part of the sulfur melting separator 14 is extruded from the top of the sulfur melting separator and enters a gas-liquid separator 16.
The shell of the sulfur melting collecting tank 15 is provided with a jacket, and steam is introduced into the jacket. Plays a role in heat preservation of the sulfur melting in the tank body, and the device is also used for the purpose of preliminary standing and precipitation of the sulfur melting liquid. The molten sulfur from the molten sulfur collecting tank 15 is sent to a molten sulfur standing tank 18.
The purpose of the gas-liquid separator 16 is to separate the incoming light liquid into water and gas, and the separated light liquid and impurities fall from the bottom of the gas-liquid separator into a waste liquid collecting tank 17 and then flow from the waste liquid collecting tank 17 to a sewage treatment plant. The separated gas is sent to a flash cooler 24.
The inside of the flash evaporation cooler 24 is provided with a washing and spraying device, the inside of the washing and circulating tank 25 is provided with filtered water, the outlet of the washing and circulating tank is used for sending water to the washing and spraying device of the flash evaporation cooler 24 through a washing pump 26, and sprayed water mist washes tail gas entering from the lower part of the flash evaporation cooler again. The washed off-gas passes through a flash cooler and is discharged from the top.
Steam is introduced into the interlayer of the shell of the molten sulfur standing tank 18 and the heating pipe inserted into the molten sulfur standing tank, so that the purposes of standing, precipitating and storing the entered molten sulfur are achieved. The molten sulfur discharged from the molten sulfur standing tank is introduced into a molten sulfur transfer tank 19.
Steam is introduced into the interlayer of the shell of the molten sulfur transfer tank 19 and the heating pipe inserted inside. A submerged pump 20 is installed inside, and the molten sulfur in the molten sulfur transfer tank 19 is sent to a pelletizer 21 by the submerged pump 20. The pelletizer 21 is a device for converting the fed molten sulfur liquid into sulfur pellets, and the fed molten sulfur is subdivided into sulfur droplets inside the pelletizer, cooled, solidified into sulfur pellets, and the sulfur pellets are fed to the packing machine 22. A baler 22 bales the fed sulphur pellets.
The invention runs the calculation of the example:
| serial number | Process for producing a metal oxide | Unit of | Data of |
| 1 | Flow of waste gas to scrubbing tower | kg/hr | 100000~125000 |
| 2 | Into a washing tower H2S content | kg/hr | 270~405 |
| 3 | Into a washing tower H2Concentration of S | ppm | 2000~3000 |
| 4 | Into a washing tower CS2Content (wt.) | kg/hr | 610~1220 |
| 5 | Into a washing tower CS2Concentration of | ppm | 2000~4000 |
| 6 | Out of washing tower H2S content | kg/hr | 7~9 |
| 7 | Out of washing tower H2Concentration of S | ppm | 60 |
| 8 | Out of washing tower CS2Content (wt.) | kg/hr | 610~1220 |
| 9 | Out of washing tower CS2Concentration of | ppm | 2000~4000 |
| 10 | Sulphur content separated from scrubber | kg/hr | 350~450 |
| 11 | Sulphur content entering sulphur heater | kg/hr | 350~450 |
| 12 | Sulfur amount of sulfur discharged from sulfur separator | kg/hr | 300~375 |
| 13 | Sulphur concentration from sulphur separator | % | 97~99 |
| 14 | Amount of sulfur separated by flash cooler and gas-liquid separator | kg/hr | 40~80 |
| 15 | Total sulfur recovery | % | 75~85 |
Claims (10)
1. A method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur is characterized in that: mixing ethylene diamine tetraacetic acid, triethanolamine, ferrous sulfate, sodium carbonate and water to prepare a washing solution; the washing solution is pumped H via a pump2S washing tower for spraying and viscose waste gas from H2S, the hydrogen sulfide gas in the viscose waste gas is absorbed by the washing solution after entering the bottom of the washing tower and fully contacting the washing solution in a countercurrent mode;
washing solution is circulated in H2S, circularly spraying in a washing tower; from H2The liquid flowing out of the bottom of the S washing column contains enriched elemental sulfur, from H2S, feeding a part of liquid flowing out of the bottom of the washing tower into a demister, and blowing air into the demister to blow off elemental sulfur foam; the foam containing the elemental sulfur is collected in a foam collecting tank and is pumped into a centrifuge through a foam conveying pump; from H2Returning the other part of the liquid from the bottom of the S washing tower to the washing liquid circulating tank, replenishing the washing solution, and pumping H2S, circularly spraying at the top of the washing tower;
the supernatant separated by the centrifuge flows back to the washing liquid circulating tank, and the separated concentrated sulfur slurry is sent to a sulfur slurry collecting tank;
soft water is added into the sulfur slurry tank and then pumped into a sulfur recovery device; heating the sulfur in a sulfur recovery device to 140 ℃ to melt the sulfur into liquid sulfur, discharging light liquid at the upper part from the top in a sulfur separator, discharging pure liquid sulfur from the bottom, sending the pure sulfur liquid to a sulfur granulator, separating the liquid into small liquid drops, cooling the liquid drops to below 50 ℃ and solidifying the liquid drops to obtain sulfur granules.
2. The method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur according to claim 1, wherein the washing solution is prepared from ethylene diamine tetraacetic acid, triethanolamine, ferrous sulfate, sodium carbonate, and water in a weight ratio of = (5 ~ 20)% (1 ~ 10)% (3 ~ 12)% (10 ~ 20)% (38 ~ 81)% by weight.
3. The method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur according to claim 1, wherein the method comprises the following steps: said H2And a hollow conical nozzle is arranged at the top of the S washing tower, and washing solution is pumped into the conical nozzle through a pump to be sprayed to absorb hydrogen sulfide gas in the viscose waste gas.
4. The method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur according to claim 1, wherein the method comprises the following steps: said H2The S washing tower has three liquid inlets, each liquid inlet is connected with H2The conical nozzles of the washing liquid sprayers inside the S washing tower are communicated, and the washing liquid flows from the H2And (S) enabling three liquid inlets on the upper part, the middle part and the lower part of the washing tower to enter three layers of spraying washing areas in the washing tower to absorb hydrogen sulfide gas in the viscose waste gas.
5. The method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur according to claim 1, wherein the method comprises the following steps: from H2S washing the liquid flowing out of the bottom of the tower, wherein 10 percent ~ 50 percent of the liquid enters a demister.
6. The method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur according to claim 1, wherein the sulfur content of the liquid in the washing liquid circulating tank is controlled to be 0.5 ~ 15.0.0 g/l, the sulfur concentration of the liquid in the foam collecting tank 8 is controlled to be 20 ~ 100g/l, and the concentration of the concentrated sulfur slurry separated by the centrifuge is 200 ~ 400 g/l.
7. The method for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur according to claim 1
The method is characterized in that soft water is added into a sulfur slurry tank, and the concentration of sulfur-containing slurry liquid is diluted to 50 ~ 200 g/l.
8. An apparatus for the method for recovering hydrogen sulfide gas from viscose waste gas to produce sulfur according to claim 1, which is characterized in that: the viscose waste gas pipeline is connected with a gas inlet at the lower part of the washing tower (1), and a gas outlet at the top of the washing tower (1) is connected with a gas inlet of the demister (2); a liquid inlet of the washing tower (1) is connected with a liquid outlet of the washing liquid circulating tank (4) through a washing liquid circulating pump (6), a washing liquid sprayer is arranged in the washing tower (1), the washing liquid sprayer is connected with a liquid inlet of the washing tower (1), and a liquid outlet at the bottom of the washing tower (1) is respectively connected with a liquid inlet of the washing liquid circulating tank (4) and a liquid inlet of the demister (5); the bottom of the demister (5) is connected with an air inlet pipe orifice, the air inlet pipe orifice is connected with an air blower (7), a discharge port at the upper part of the demister (5) is connected with a feed port of a foam collecting tank (8), and the discharge port of the foam collecting tank (8) is connected with a feed port of a centrifugal machine (10) through a foam delivery pump (9); the discharge hole of the centrifuge (10) is connected with the feed hole of the sulfur slurry collecting tank (11); a discharge port of the sulfur slurry collecting tank (11) is connected with a feed port at the top of the sulfur heater (13) through a sulfur slurry conveying pump (12); an upper liquid outlet and a lower discharge outlet of the sulfur heater (13) are respectively connected with an upper liquid inlet and a bottom feed inlet of the sulfur melting separator (14); a discharge hole at the lower part of the sulfur melting separator (14) is connected with a sulfur melting collecting tank (15), and a waste liquid discharge hole at the top of the sulfur melting separator (14) is connected with a feed hole of a gas-liquid separator (16); a discharge hole at the lower part of the molten sulfur collecting tank (15) is connected with a feed hole of the molten sulfur standing tank (18); a discharge port at the upper part of the molten sulfur standing tank (18) is connected with a feed port of a molten sulfur transfer tank (19).
9. Treatment of H from viscose waste gas according to claim 82S retrieves device of sulphur, its characterized in that: the liquid inlet of the washing tower (1) is an upper liquid inlet, a middle liquid inlet and a lower liquid inlet, three washing liquid sprayers are arranged in the washing tower (1), and the three washing liquid sprayers are respectively connected with the respective corresponding liquid inlets;
a branch of a liquid inlet above the washing tower (1) is connected with a liquid outlet of the washing liquid preparation tank (23); an air outlet at the side part of the demister (2) is connected with a demisting fan (3), and a liquid outlet at the bottom part is connected with a liquid inlet of the demister (5);
the overflow port of the demister (5) is connected with the liquid inlet of the washing liquid circulating tank (4).
10. Treatment of H from viscose waste gas according to claim 82S retrieves device of sulphur, its characterized in that: a liquid outlet at the bottom of the gas-liquid separator (16) is positioned above the waste liquid collecting pool (17), and an exhaust port at the top of the gas-liquid separator (16) is connected with an air inlet at the lower part of the flash evaporator (24); the exhaust port at the top of the flash evaporation cooler (24) is connected with the atmosphere, the water inlet at the upper part of the flash evaporation cooler (24) is connected with the water washing circulating tank (25) through the water washing pump (26), the water inlet of the flash evaporation cooler (24) is connected with the internal washing sprayer, the water outlet at the bottom of the flash evaporation cooler (24) is connected with the water washing circulating tank (25), and the water inlet of the water washing circulating tank (25) is connected with the filtering water pipeline.
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| CN201910078067.XA CN110655042A (en) | 2019-01-28 | 2019-01-28 | Method and device for recovering hydrogen sulfide gas from viscose waste gas to prepare sulfur |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112062101A (en) * | 2020-09-30 | 2020-12-11 | 中石化石油工程技术服务有限公司 | Energy-saving continuous sulfur melting device and process thereof |
| CN112973384A (en) * | 2021-02-05 | 2021-06-18 | 杭州九木环境有限公司 | Treatment of H-containing materials with iron chelate2S and CS2Apparatus and method for exhaust gas |
| CN114426261A (en) * | 2022-01-27 | 2022-05-03 | 济南冶金化工设备有限公司 | System and process for producing sulfur paste powder by dehydrating and drying sulfur foam |
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| CN112062101A (en) * | 2020-09-30 | 2020-12-11 | 中石化石油工程技术服务有限公司 | Energy-saving continuous sulfur melting device and process thereof |
| CN112973384A (en) * | 2021-02-05 | 2021-06-18 | 杭州九木环境有限公司 | Treatment of H-containing materials with iron chelate2S and CS2Apparatus and method for exhaust gas |
| CN114426261A (en) * | 2022-01-27 | 2022-05-03 | 济南冶金化工设备有限公司 | System and process for producing sulfur paste powder by dehydrating and drying sulfur foam |
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Application publication date: 20200107 |