CN102277205A - Method for extracting salt from coke oven gas by desulfuration and decyanation - Google Patents
Method for extracting salt from coke oven gas by desulfuration and decyanation Download PDFInfo
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Abstract
The invention discloses a method for extracting salt from coke oven gas by desulfuration and decyanation. The method provided by the invention comprises the following steps of: (1) transferring the coke oven gas into a lower part of a desulfuration system and contacting the gas with sprayed absorbing barren liquor; discharging purified gas from the top part of the desulfuration system and transferring added strong aqua ammonia into the desulfuration system from a bottom storing tank of the desulfuration system; (2) adding an organic compound catalyst into absorbing rich liquor discharged from the desulfuration system; pressurizing and cooling; adding the mixture and compressed air into the bottom of an oxidizing system; then transferring the absorbing barren liquor from the upper part of the oxidizing system into the desulfuration system again and transferring a portion of the liquor into a subsequent salt-extracting procedure; (3) purifying exhaust gas from the oxidizing gas and then discharging; (3) heating the absorbing barren liquor which is transferred to the subsequent recycling work section, evaporating and concentrating in vacuum, filtering and collecting crude ammonium thiosulfate; and (4) collecting crude ammonium thiocyanate from the filtering solution obtained by the step (3). According to the method provided by the invention, the desulfuration rate can reach more than 99%, the decyanation can reach more than 90% and the additional value of the product is high.
Description
Technical field
The present invention relates to the purifying method of coke-oven gas.
Background technology
There is the arsenic alkaline process in China in 50～sixties, ammonia liquor catalysis process and domestic Nan Huayuan, chemical plant, Sichuan and Wusong producer gas plant are developed jointly out improvement ADA method in early 1960s.But these methods always have such or such shortcoming, and for example the arsenic alkaline process is too big owing to containing arsenic alkali solution toxicity, and the mankind are endangered greatly, is eliminated.Ammonia liquor catalysis process, main catalyzer is a Resorcinol, and is active relatively poor, and sulphur is too thin, easily stifled tower, this method is undesirable.Increase for example PDS of Northeast Normal University's exploitation of other catalyzer afterwards again, progressively developed into the HPF method of the common exploitation of coke-oven plant, Wuxi and Anshan Jiao Nai institute later on.Though improvement ADA method is still being used, its technical process is long, and the production sulfur environment is poor.Production cost height, desulfurization waste liquor are handled difficult, so there be limited evidence currently of uses.
Since last century the eighties successively be called for short (VS-Crouse or WSA method) and add HPF method (the similar ZL of having method, PDS method etc.), the OPT method of Anshan Thermal Energy Inst.'s exploitation nineties in 20th century from FRC method (three phases of Baosteel), vacuum carbonate-sulphur or the sulfuric acid process of the MEA-sulfuric acid process (Baosteel second phase) of the AS method of the external Ta Xifa that introduces Nippon Steel (Baosteel first phase), Thyssen company, NKK, Osaka Gas Company.The coke-oven-gas desulfurization and decyanation technology production technology has obtained sizable progress.But still there is deficiency in these methods, adopt the high-voltage wet type oxidation as the Ta Xifa liquid waste disposal, and after the High Temperature High Pressure wet oxidation, used heat vapour does not make full use of, and causes power consumption big, and the reaction tower manufacture difficulty is big, difficult the popularization; AS method desulfuration and decyanation efficient is not too high, and operations such as desulfuration and decyanation, deamination, ammonia still process and sulfur recovery must connect together, and go wrong and will influence the production of whole desulfuration and decyanation in the part, and economic benefit is bad.VS-WAS method and AS method are similar, and desulfuration and decyanation efficient own is not too high, investment is big, economic benefit is bad.The back desulfurization owned by France of MEA-sulfuric acid, MEA, the big running cost height of steam consumption, deficiency in economic performance.The FRC method is a stainless steel equipment because technical process is long entirely, and investment is big, and the operation of equipment difficulty is big, except that three phase of Baosteel coal gas is refining use, domestic do not have ordinary production enterprise so far as yet; HPF method (comprising ZL method, PDS etc.) exists production sulphur or sulphur cream environment poor, produces a large amount of waste liquids, deficiencies such as severe corrosion equipment and contaminate environment.The OPT method also is to produce sulphur cream, and same environment is poor, and sulfur granule is thin in the doctor solution, easily stifled tower, but owing to there is liquid waste treating apparatus can obtain byproducts such as ammonium thiocyanate, ammonium thiosulfate, economic benefit, environmental protection situation slightly are better than the HPF method.
Summary of the invention
The purpose of this invention is to provide a kind of method that efficiently removes and reclaim hydrogen sulfide and prussic acid from coke-oven gas, do not produce sulphur cream and sulphur, reclaim ammonium thiocyanate, ammonium thiosulfate in the desulfurization waste liquor, waste gas all purifies recovery, to overcome the defective that prior art exists, satisfy the needs of relevant branch of industry.
Method of the present invention comprises the steps:
(1) coke-oven gas that will need to handle is sent into the desulphurization system bottom, contacts with the absorption lean solution that the desulphurization system top spray gets off, and absorbs hydrogen sulfide and prussic acid in the coal gas;
In the described coke-oven gas, hydrogen sulfide content is 4～10g/m
3, hydrogen cyanide content is 1～2.0g/m
3, absorption temperature is 20～38 ℃, liquid (weight t)/gas (volume m
3) than being 1: 1～1.2;
Coal gas after the purification is discharged by the desulphurization system top, is sent to follow-up workshop section;
The strong aqua that replenishes storage tank at the bottom of the desulphurization system enters desulphurization system, and the weight concentration of described additional strong aqua is 10%～16%;
Described absorption lean solution is the ammonia soln that contains salt, and the weight concentration of ammonia is 7～20g/L, and the concentration of salt is 200～300g/L;
Described salt is ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate, and weight ratio is:
Ammonium thiocyanate: ammonium thiosulfate: ammonium sulfate=1: 1.2～1.5: 0.08～0.12;
(2) go out the absorption rich solution of desulphurization system, add organic composite catalyst, pressurization postcooling to temperature is 30～38 ℃, and then sends into the oxidation system bottom with pressurized air, makes ammonia, hydrogen sulfide and prussic acid in the rich solution change into ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate;
Absorb rich solution and compressed-air actuated liquid (weight t)/gas (volume m
3) than being 1: 1～1.2, working pressure is 15000～20000pa;
Described organic composite catalyst is made up of following components in weight percentage:
1,4-naphthoquinones-2-sodium sulfonate 85～90%
Resorcinol 5～10%
Ammonium oxalate 3～10%.
Described 1,4-naphthoquinones-2-sodium sulfonate can adopt commercially produced product, as the product of Kawasaki, Japan chemical company;
Described Resorcinol can adopt commercially produced product, as the product of the auspicious chemical industry in sky, Zhengzhou company limited;
Organic composite catalyst is a catalysts, absorbs in the rich solution, and its content is 0.2～0.3ppm;
Absorption lean solution part after coming out from oxidation system top enters desulphurization system once more, recycles, and part is sent to the follow-up salt operation of putting forward;
The absorption lean solution that enters desulphurization system is 1000～1600: 1 with the weight ratio that is sent to the follow-up absorption lean solution of putting forward the salt operation, and wherein, the concentration of salt is 200～300g/L;
Be sent to follow-up exhaust gas purification system from oxidation system top tail gas discharged and purify the back discharging;
Further, the present invention also comprises:
(3) be sent to the follow-up absorption lean solution of putting forward the salt operation after will coming out from oxidation system top, be heated to 50～90 ℃, after the filtration, filtrate is sent into the ammonium thiosulfate evaporation and crystallization system, it is under the condition of 0.08～0.1Mpa with vacuum tightness that filtrate is 52～70 ℃ in temperature, carrying out vacuum-evaporation concentrates, be evaporated to solution proportion ρ=1.280～1.320, the slurries ratio is 30～50% o'clock, acquisition contains thick ammonium thiosulfate crystalline solution, send into the ammonium thiosulfate centrifugal separation system, filter, collect filter cake, be thick ammonium thiosulfate, be sent to follow-up ammonium thiosulfate refining step;
(4) filtrate of step (3) acquisition is sent into the ammonium thiocyanate crystal system, is to carry out crystallization under 20～25 ℃ in temperature, when the crystalline substance ratio reaches 30～50%, filters, collects filter cake, is thick ammonium thiocyanate, is sent to follow-up ammonium thiocyanate refining step.
Major advantage of the present invention:
Adopt method of the present invention, remove hydrogen sulfide and prussic acid in the coke-oven gas, desulfuration efficiency height, H behind the tower
2S≤100mg/m
3', desulfuration efficiency reaches more than 99%; Decyanation efficient height, coal gas contains HCN≤150mg/m behind the tower
3, decyanation efficient reaches 90%, the added value of product height, and energy consumption is low, comprehensive energy consumption is than HPF, and the VS-WSA method is all low, with remained ammonia with add organic composite catalyst and make catalyzer, convenient sources, expense is minimum, and technology is simple, and equipment is less, reduced investment, productive expense is minimum, and labour intensity is low, produces and stablizes, and maintenance capacity is little, and various energy consumptions, raw materials consumption is few, so productive expense is minimum, do not produce sulfur product in the production process, avoided production sulphur cream like this, environmental pollution during molten sulfur.All waste gases is all handled the back discharging through cleaning.Do not discharge any liquid, secondary salt is converted into high ammonium thiosulfate of added value and ammonium thiocyanate, delivers to coal yard after minute quantity coal dust, coke powder reclaim and utilizes.So can build up cleaning garden device.The desulphurization system turndown ratio is big, and 25%～100% all can operate; The doctor solution saltiness can be adjusted according to ammonia, hydrogen sulfide, hydrogen cyanide content fluctuation in the coal gas, and the turndown ratio of carrying salt is big.
Description of drawings
Fig. 1 is a schema of the present invention.
Embodiment
Referring to Fig. 1, method of the present invention comprises the steps:
(1) coke-oven gas that will need to handle is sent into desulphurization system 1 bottom, and the absorption lean solution that spray with desulphurization system 1 top contacts, hydrogen sulfide and prussic acid in the absorption coal gas;
Coal gas after the purification is discharged by desulphurization system 1 top, is sent to follow-up workshop section;
The strong aqua that replenishes enters desulphurization system 1 from the end storage tank of desulphurization system 1;
(2) go out the absorption rich solution pressurization cooling of desulphurization system 1 after, send into oxidation system 2 bottoms with pressurized air again;
Absorption lean solution part after coming out from oxidation system 2 tops enters desulphurization system 1 once more, recycles, and part is sent to the follow-up salt operation of putting forward;
Be sent to follow-up exhaust gas purification system 7 purification back dischargings from the top tail gas discharged of oxidation system 2;
(3) after will coming out from the top of oxidation system 2 be sent to the follow-up absorption lean solution heating and filtering of putting forward the salt operation after, filtrate is sent into ammonium thiosulfate evaporation and crystallization system 3, carrying out vacuum-evaporation concentrates, acquisition contains thick ammonium thiosulfate crystalline solution, send into ammonium thiosulfate centrifugal separation system 4, filter, collect filter cake, be thick ammonium thiosulfate, be sent to follow-up ammonium thiosulfate refining step;
(4) filtrate that obtains of step (3) is sent into ammonium thiocyanate crystal system 5, carries out crystallization, reach regulation brilliant than after, send into ammonium thiocyanate centrifugal separation system 6, filter, collect filter cake, be thick ammonium thiocyanate, be sent to follow-up ammonium thiocyanate refining step.
Further, can adopt two or more desulphurization system, connect or parallel operation, this is also within protection scope of the present invention.
Embodiment 1
Adopt the flow process of Fig. 1.The basic technology parameter is as follows:
Coke-oven gas tolerance is 28000m
3/ h, wherein, hydrogen sulfide content is 4.612g/m
3, hydrogen cyanide content is 1.233g/m
3
Absorbing the lean solution flow is 1200t/h, and wherein: the weight concentration of ammonia is 7g/L, and the concentration of salt is 200g/L;
Salt is ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate, and weight ratio is:
Ammonium thiocyanate: ammonium thiosulfate: ammonium sulfate=1: 1.5: 0.12;
Absorption temperature is 38 ℃, absorbs rich solution and compressed-air actuated liquid (weight t)/gas (volume m
3) than being 1: 1;
In the coal gas after the purification, the content of hydrogen sulfide is 0.024g/m
3, hydrogen cyanide content is 0.097g/m
3The weight concentration of the strong aqua that replenishes is 16%; Magnitude of recruitment is 1.5t/h;
The organic composite catalyzing agent content that adds in the absorption rich solution of thionizer is 0.3ppm, and pressurization postcooling to temperature is 38 ℃, and then sends into the oxidizing tower bottom with pressurized air;
The weight percent of organic composite catalyst consists of:
1,4-naphthoquinones-2-sodium sulfonate 85%, Resorcinol 10%, ammonium oxalate 5%.
Working pressure is 15000pa, air supply 1200m
3/ h absorbs rich solution and compressed-air actuated liquid (weight t)/gas (volume m
3) than being 1: 1;
Absorption lean solution part after coming out from oxidizing tower top enters thionizer once more, recycles, and part is sent to the follow-up salt operation of putting forward; The absorption lean solution that enters thionizer is 1000: 1 with the weight ratio that is sent to the follow-up absorption lean solution of putting forward the salt operation, and wherein, the concentration of salt is 200g/L;
(4) be sent to the absorption lean solution of follow-up recycle section, be heated to 90 ℃, after the filtration, it is under the condition of 0.1Mpa with vacuum tightness that filtrate is 70 ℃ in temperature, vacuum-evaporation concentrates, be evaporated to solution proportion ρ=1.320, the slurry weight ratio is 50% o'clock, filters, collects filter cake, is thick ammonium thiosulfate;
(5) filtrate that step (4) is obtained is to carry out crystallization under 25 ℃ in temperature, when the crystalline substance ratio reaches 50%, filters, collects filter cake, is thick ammonium thiocyanate.
Desulfuration efficiency is 99.48%, and decyanation efficient is 92.13%.
Adopt the flow process of Fig. 1.The basic technology parameter is as follows:
Coke-oven gas tolerance is 100000m
3/ h, wherein, hydrogen sulfide content is 9.5g/m
3, hydrogen cyanide content is 1.8g/m
3
Absorbing the lean solution flow is 4200t/h, and wherein: the weight concentration of ammonia is 20g/L, and the concentration of salt is 300g/L;
Salt is ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate, and weight ratio is:
Ammonium thiocyanate: ammonium thiosulfate: ammonium sulfate=1: 1.2: 0.08;
Absorption temperature is 30 ℃, absorbs rich solution and compressed-air actuated liquid (weight t)/gas (volume m
3) than being 1: 1.2
In the coal gas after the purification, the content of hydrogen sulfide is 0.092g/m
3, hydrogen cyanide content is 0.120g/m
3The weight concentration of the strong aqua that replenishes is 10%; Magnitude of recruitment is 5t/h;
The organic composite catalyzing agent content that adds in the absorption rich solution of thionizer is 0.2ppm, and pressurization postcooling to temperature is 30 ℃, and then sends into the oxidizing tower bottom with pressurized air;
Organic composite catalyst consists of: 1, and 4-naphthoquinones-2-sodium sulfonate 90%, Resorcinol 5%, ammonium oxalate 5%.
Working pressure is 20000Pa; Air supply 5000m
3/ h;
Absorption lean solution part after coming out from oxidizing tower top enters thionizer once more, recycles, and part is sent to the follow-up salt operation of putting forward; The absorption lean solution that enters thionizer is 1000: 1 with the weight ratio that is sent to the follow-up absorption lean solution of putting forward the salt operation, and wherein, the concentration of salt is 300g/l;
(4) be sent to the absorption lean solution of follow-up recycle section, be heated to 50 ℃, after the filtration, it is under the condition of 0.08Mpa with vacuum tightness that filtrate is 52 ℃ in temperature, vacuum-evaporation concentrates, be evaporated to solution proportion ρ=1.280, the slurry weight ratio is 30% o'clock, filters, collects filter cake, is thick ammonium thiosulfate;
(5) filtrate that step (4) is obtained is to carry out crystallization under 20 ℃ in temperature, when the crystalline substance ratio reaches 30%, filters, collects filter cake, is thick ammonium thiocyanate.
Desulfuration efficiency is 99.03%, and decyanation efficient is 93.33%.
Claims (11)
- One kind from coke-oven gas desulfuration and decyanation put forward the method for salt, it is characterized in that, comprise the steps:(1) coke-oven gas that will need to handle is sent into the desulphurization system bottom, contacts with the absorption lean solution that the desulphurization system top spray gets off, and absorbs hydrogen sulfide and prussic acid in the coal gas;Coal gas after the purification is discharged by the desulphurization system top, is sent to follow-up workshop section;The strong aqua that replenishes storage tank at the bottom of the desulphurization system enters desulphurization system;Described absorption lean solution is the ammonia soln that contains salt;(2) go out the absorption rich solution of desulphurization system, add organic composite catalyst, the pressurization postcooling is sent into the oxidation system bottom with pressurized air then;Absorption lean solution part after coming out from oxidation system top enters desulphurization system once more, recycles, and part is sent to the follow-up salt operation of putting forward;Be sent to follow-up exhaust gas recovery system from oxidation system top tail gas discharged and purify the back discharging.
- 2. method according to claim 1 is characterized in that, in the described coke-oven gas, hydrogen sulfide content is 4～10g/m 3, hydrogen cyanide content is 1～2.0g/m 3
- 3. method according to claim 1 is characterized in that, absorption temperature is 20～38 ℃, liquid (weight t)/gas (volume m 3) than being 1: 1～1.2.
- 4. method according to claim 1 is characterized in that, the weight concentration of described strong aqua is 10%～16%.
- 5. method according to claim 1 is characterized in that, described absorption lean solution is the ammonia soln that contains salt, and the concentration of ammonia is 7～20g/L, and the concentration of salt is 200～300g/L;Described salt is ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate, and weight ratio is:Ammonium thiocyanate: ammonium thiosulfate: ammonium sulfate=1: 1.2～1.5: 0.08～0.12.
- 6. method according to claim 1 is characterized in that, absorbs rich solution and compressed-air actuated liquid (weight t)/gas (volume m 3) than being 1: 1～1.2, working pressure is 15000～20000pa.
- 7. according to the described method of claim 1, it is characterized in that absorb in the rich solution, organic composite catalyzing agent content is 0.2～0.3ppm.
- 8. according to the described method of claim 1, it is characterized in that the absorption lean solution that enters thionizer is 1000～1600: 1 with the weight ratio that is sent to the follow-up absorption lean solution of putting forward the salt operation, wherein, the concentration of salt is 200～300g/L.
- 9. according to each described method of claim 1～8, it is characterized in that, also comprise step down:(3) be sent to the follow-up absorption lean solution of putting forward the salt operation after will coming out from oxidation system top, be heated to 50～90 ℃, after the filtration, filtrate is that 52～70 ℃ and vacuum tightness are under the condition of 0.08～0.1Mpa in temperature, carries out vacuum-evaporation and concentrates, and is evaporated to solution proportion ρ=1.280～1.320, the slurries ratio is at 30～50% o'clock, acquisition contains thick ammonium thiosulfate crystalline solution, filter, collect filter cake, be thick ammonium thiosulfate, be sent to follow-up ammonium thiosulfate refining step.
- 10. method according to claim 9 is characterized in that, also comprises the steps:(4) filtrate of step (3) acquisition is to carry out crystallization under 20～25 ℃ in temperature, when the crystalline substance ratio reaches 30～50%, filters, collects filter cake, is thick ammonium thiocyanate, is sent to follow-up ammonium thiocyanate refining step.
- 11. method according to claim 9 is characterized in that, described organic composite catalyst is consisted of by following components in weight percentage: 1, and 4-naphthoquinones-2-sodium sulfonate is 85～90%, and Resorcinol is 5～10%, and ammonium oxalate is 3～10%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107352679A (en) * | 2017-07-11 | 2017-11-17 | 河南中鸿集团煤化有限公司 | A kind of doctor solution salt extraction technique and its device |
| CN109852434A (en) * | 2019-02-20 | 2019-06-07 | 宁波科新化工工程技术有限公司 | A kind of method of coke-oven-gas desulfurization and decyanation concentration relieving haperacidity |
| CN107804829B (en) * | 2017-07-27 | 2023-10-20 | 杨承诣 | Method for preparing sulfur dioxide by utilizing byproducts of desulfurization system in coking industry |
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|---|---|---|---|---|
| CN101333464A (en) * | 2008-08-04 | 2008-12-31 | 马永伟 | Desulphurization process by vacuum ammonia method |
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2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333464A (en) * | 2008-08-04 | 2008-12-31 | 马永伟 | Desulphurization process by vacuum ammonia method |
Non-Patent Citations (1)
| Title |
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| 缪兆良 等: "YST脱硫脱氰工艺的生产实践", 《燃料与化工》, vol. 41, no. 1, 31 January 2010 (2010-01-31) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107352679A (en) * | 2017-07-11 | 2017-11-17 | 河南中鸿集团煤化有限公司 | A kind of doctor solution salt extraction technique and its device |
| CN107352679B (en) * | 2017-07-11 | 2022-01-07 | 河南中鸿集团煤化有限公司 | Desulfurization liquid salt extraction process and device thereof |
| CN107804829B (en) * | 2017-07-27 | 2023-10-20 | 杨承诣 | Method for preparing sulfur dioxide by utilizing byproducts of desulfurization system in coking industry |
| CN109852434A (en) * | 2019-02-20 | 2019-06-07 | 宁波科新化工工程技术有限公司 | A kind of method of coke-oven-gas desulfurization and decyanation concentration relieving haperacidity |
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