CN104449881A - Method for purifying coke oven gas of vacuum carbonate-process desulphurization and recovering sodium thiocyanate - Google Patents
Method for purifying coke oven gas of vacuum carbonate-process desulphurization and recovering sodium thiocyanate Download PDFInfo
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- CN104449881A CN104449881A CN201410203103.8A CN201410203103A CN104449881A CN 104449881 A CN104449881 A CN 104449881A CN 201410203103 A CN201410203103 A CN 201410203103A CN 104449881 A CN104449881 A CN 104449881A
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- oven gas
- sodium thiocyanate
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
- C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/20—Thiocyanic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/04—Purifying combustible gases containing carbon monoxide by cooling to condense non-gaseous materials
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
- C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
- C10K1/12—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids alkaline-reacting including the revival of the used wash liquors
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
- C10K1/16—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with non-aqueous liquids
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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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- Life Sciences & Earth Sciences (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention relates to a method for purifying the coke oven gas of vacuum carbonate-process desulphurization and recovering sodium thiocyanate. The method comprises the following steps of cooling, cleaning tar, washing ammonia, removing benzene, removing oil, removing naphthalene and the like, and further comprises the step of recovering sodium cyanate from desulphurization and decyanation wastewater, and the step comprises the following specific steps: 1) adding active carbon; 2) filtering; 3) extracting and crystallizing; and 4) refining, and returning the mother liquor obtained by separation to an evaporator. According to the method disclosed by the invention, the treatment process is simplified, repeated recrystallization is avoided, and the treatment cost is greatly reduced, so that the recovered by-products achieve the requirements of industrial high-grade products, the energy consumption is greatly reduced, zero emission is really realized, and the requirement of green and cyclic economy is achieved.
Description
Technical field
The present invention relates to coke oven gas purification and waste water utilization field, particularly a kind of coke oven gas purification of vacuum carbonate desulphurization and the method for recovery Sodium Thiocyanate 99.
Background technology
Vacuum carbonation coke-oven-gas desulfurization and decyanation technology belongs to wet absorption method sulfur removal technology.Its main technique first adopts carbonate solution directly to absorb hydrogen sulfide in coal gas and prussic acid; The rich solution absorbing sour gas enters regenerator column regeneration, and contact with the water vapor risen at the bottom of regenerator column under vacuum with cold condition, sour gas desorbs from rich solution; The sour gas produced can adopt Kraus process to produce elementary sulfur or adopt contact process to produce sulfuric acid.Carry out in the process of coke-oven-gas desulfurization and decyanation in employing vacuum carbonation, the waste liquid containing high density prussiate and sulfide can be produced.This waste liquid forms primarily of two portions, and the part that wherein quantity discharged is larger is vacuum condensation liquid, and it is when sour gas vacuum condensation because water vapor condensation wherein produces, and its main component is cyanide salt and sulphide salt, colourless, pH7 ~ 8; Another part that quantity discharged is less is carbonate lean solution, it needs a small amount of discharge for preventing impurity enriched in carbonate lean solution from affecting prussic acid and hydrogen sulfide absorption, and its main component is carbonate, cyanide salt and sulphide salt, also containing the organism such as tar, phenol, sorrel, about pH10.
In coke-oven plant, the desulfuration and decyanation waste liquid that usual vacuum potassium carbonate method produces directly enters coking chemical waste water biochemical treatment system to process, but because prussiate wherein and sulfide content are all very high, up to thousands of to mg/L up to ten thousand, directly enter coking chemical waste water biochemical treatment system and can produce very large restraining effect to its biological activity, biological treatment system treatment effect is caused lowly even to paralyse, make water outlet can not qualified discharge, this just need desulfuration and decyanation waste liquid to carry out processing make prussiate wherein and sulfide be reduced to the level not affecting biological treatment after can enter biochemical treatment system and be further processed.
Because the prussiate in waste water and sulfide content are all higher, by two steps respectively precipitated sulfur compound and prussiate have any problem, and to remove by acid adding the process of acid waste water containing a large amount of sulfide that impurity produces also be very large problem.
Summary of the invention
The object of this invention is to provide the coke oven gas purification of vacuum carbonate desulphurization and reclaim the method for Sodium Thiocyanate 99, spray catcher trapping weak effect after benzene tower is washed to solve in prior art, cause the impurity such as washing oil in coke-oven gas, tar, naphthalene to enter follow-up desulphurization system, cause the technical problem of regenerator column, vacuum pump frequent jams.
The present invention solves the problems of the technologies described above by the following technical programs.
A purifying method for the coke-oven gas of matched with vacuum carbonate desulphurization, comprises the following steps:
A), raw gas is sent into primary cooler and cool to 22 DEG C;
B) coke-oven gas, step a) processed is sent into electrical tar precipitator and is removed tar fog;
C), by step b) coke-oven gas that processed sends into gas blower and is warmed up to 37 DEG C;
D), by step c) coke-oven gas that processed sends into pickling tower and washes ammonia, and after completing, temperature drops to 25 DEG C;
E), by steps d) coke-oven gas that processed sends into and washes benzene tower washing oil and take off benzene, and now temperature is 27 DEG C;
F), by step e) coke-oven gas that processed sends into water wash column washings and sprays and remove washing oil, tar, naphthalene further;
G) coke-oven gas, after above-mentioned steps purification enters desulphurization system, carries out vacuum carbonate desulphurization technique, obtains 30 DEG C of purified gas.
Preferably, step f) in washings be service water or distilled ammonia wastewater, water wash column circulation fountain height controls at 25 ~ 30m
3/ 10000m
3coal gas.
Preferably, in step g), the thionizer top of desulphurization system increases NaOH washing section, can make H in coal gas
2the content of S is down to 0.2g/m
3below.
From the waste water that above-mentioned technique produces, reclaim a method for Sodium Thiocyanate 99, its step comprises:
1) activated carbon decolorizing, activated carbon dosage is 0.3 ~ 1% of wastewater treatment capacity, temperature condition 10 ~ 30 DEG C;
2) filter destainer, obtain clear liquid and waste active carbon, waste active carbon returns coal yard and enters pit kiln, and the water of condensation produced in decolorization enters condenser cooling and reclaims;
3) extractive crystallization process is adopted to extract Sodium Thiocyanate 99 from desulfurization waste liquor, adopt continuous cooling crystallizer, cool under 35 DEG C of conditions, then solid-liquor separation is carried out with whizzer, being separated the purity obtaining solid sulfur Zassol NaSCN is 97%, and also comprise sodium sulfate, Sulfothiorine, concentrate feed separation temperature after crystallisation by cooling controls at 30 ~ 40 degree, be separated finished product Sodium Thiocyanate 99 with crystal water lower than 30 degree, cause finished product content to reduce;
4) Sodium Thiocyanate 99 is refined, and adopt recrystallization method to obtain fine work Sodium Thiocyanate 99 NaSCN purity and be greater than 99.5%, in Sodium Thiocyanate 99, chloride ion content is less than 0.01%;
5) extraction liquid is got back to vaporizer and is evaporated.
Preferably, in step 3), the temperature of cooling crystallizer is controlled by cooling water inflow.
Preferably, in step 5), vaporizer adopts triple-effect evaporator, reducing, keeping the necessary temperature difference for maintaining its evaporator room pressure by effect.The a small amount of sodium sulfate of residue after process is as fixed-end forces.
Preferably, the water produced in above each step is got back to previous cycles and is used.
The present invention adopts totally-enclosed recycling, utilizes, simplify treating processes to waste liquid circulation, avoid recrystallization repeatedly, processing cost reduces greatly, makes the byproduct of recovery reach the requirement of technical grade top grade product, greatly reduce energy consumption, really accomplish zero release, reach green circulation economy requirement.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with embodiment.
The coke oven gas purification method of vacuum carbonate desulphurization, the steps include: raw gas → cooling → electrically trapped tar oil → gas blower → wash ammonia → de-benzene → de-oiling, de-naphthalene → desulfurization → purified gas.This sulfur removal technology desulfuration efficiency is high, increases NaOH washing section, can make H in coal gas on thionizer top
2the content of S is down to 0.2g/m
3below, coal chemical enterprise requirements for sale can be met.To produce sulfur conversion rate high, Claus tail gases return inhale gas line can not atmosphere pollution, and the hot water that the thermal source available waste heat boiler for producing steam of regenerator column and primary cooler produce all can utilize, therefore UTILIZATION OF VESIDUAL HEAT IN is good.
From the waste water that above-mentioned technique produces, reclaim the method for Sodium Thiocyanate 99, its step comprises:
1) activated carbon decolorizing, activated carbon dosage is 0.3 ~ 1% of wastewater treatment capacity, temperature condition 10 ~ 30 DEG C.
2) Plate Filtration, activated carbon goes regeneration, secondary filter, and solution is as clear as crystal, and waste active carbon returns coal yard and enters pit kiln, and the water of condensation produced in decolorization enters condenser cooling and reclaims.
3) extractive crystallization process is adopted to extract Sodium Thiocyanate 99 from desulfurization waste liquor, adopt continuous cooling crystallizer, cool under 35 DEG C of conditions, then solid-liquor separation is carried out with whizzer, being separated the purity obtaining solid sulfur Zassol NaSCN is 97%, and also comprise sodium sulfate, Sulfothiorine, concentrate feed separation temperature after crystallisation by cooling controls at 30 ~ 40 degree, be separated finished product Sodium Thiocyanate 99 with crystal water lower than 30 degree, cause finished product content to reduce.The temperature of cooling crystallizer is mainly controlled by cooling water inflow.
4) Sodium Thiocyanate 99 is refined, and adopt recrystallization method to obtain fine work Sodium Thiocyanate 99 NaSCN purity and be greater than 99.5%, in Sodium Thiocyanate 99, chloride ion content is less than 0.01%, and quality product can reach premium grads.
5) extraction liquid is got back to vaporizer and is evaporated.Evaporation adopts triple-effect evaporator, energy efficient.Maintaining vacuum operating can make vaporization temperature reduce, and improves production intensity further and reduces solution to the corrosive environment of material.Multi-effect evaporation system reduces by effect for maintaining its evaporator room pressure, and keep the necessary temperature difference, its end effect must be connected with vacuum unit.
Those of ordinary skill in the art will be appreciated that, above embodiment is only used to the present invention is described, and be not used as limitation of the invention, as long as in spirit of the present invention, all will the present invention be dropped on to the change of the above embodiment, modification.
Claims (8)
1. the coke oven gas purification method of vacuum carbonate desulphurization, is characterized in that, comprise the following steps:
A), raw gas is sent into primary cooler and cool to 22 DEG C;
B) coke-oven gas, step a) processed is sent into electrical tar precipitator and is removed tar fog;
C), by step b) coke-oven gas that processed sends into gas blower and is warmed up to 37 DEG C;
D), by step c) coke-oven gas that processed sends into pickling tower and washes ammonia, and after completing, temperature drops to 25 DEG C;
E), by steps d) coke-oven gas that processed sends into and washes benzene tower washing oil and take off benzene, and now temperature is 27 DEG C;
F), by step e) coke-oven gas that processed sends into water wash column washings and sprays and remove washing oil, tar, naphthalene further;
G) coke-oven gas, after above-mentioned steps purification enters desulphurization system, carries out vacuum carbonate desulphurization technique, obtains 30 DEG C of purified gas;
From wastewater for desulfurization and decyanation, reclaim Sodium Thiocyanate 99 further, comprise following steps:
1) activated carbon decolorizing, activated carbon dosage is 0.3 ~ 1% of wastewater treatment capacity, temperature condition 10 ~ 30 DEG C;
2) filter destainer, obtain clear liquid and waste active carbon, waste active carbon returns coal yard and enters pit kiln, and the water of condensation produced in decolorization enters condenser cooling and reclaims;
3) extractive crystallization process is adopted to extract Sodium Thiocyanate 99 from desulfurization waste liquor, adopt continuous cooling crystallizer, cool under 35 DEG C of conditions, then solid-liquor separation is carried out with whizzer, being separated the purity obtaining solid sulfur Zassol NaSCN is 97%, also comprise sodium sulfate, Sulfothiorine, concentrate feed separation temperature after crystallisation by cooling controls at 30 ~ 40 degree;
4) Sodium Thiocyanate 99 is refined, and adopt recrystallization method to obtain fine work Sodium Thiocyanate 99 NaSCN purity and be greater than 99.5%, in Sodium Thiocyanate 99, chloride ion content is less than 0.01%;
5) extraction liquid is got back to vaporizer and is evaporated.
2. vacuum carbonate desulphurization according to claim 1 coke oven gas purification and reclaim the method for Sodium Thiocyanate 99, it is characterized in that: described step f) in washings be service water or distilled ammonia wastewater.
3. the coke oven gas purification of vacuum carbonate desulphurization according to claim 1 and the method for recovery Sodium Thiocyanate 99, is characterized in that: in described step f), water wash column circulation fountain height controls at 25 ~ 30m
3/ 10000m
3coal gas.
4. the coke oven gas purification of vacuum carbonate desulphurization according to claim 3 and the method for recovery Sodium Thiocyanate 99, is characterized in that: in described step 3), the temperature of cooling crystallizer is controlled by cooling water inflow.
5. the coke oven gas purification of vacuum carbonate desulphurization according to claim 1 and the method for recovery Sodium Thiocyanate 99, is characterized in that: in described step g), the thionizer top of desulphurization system increases NaOH washing section, H in coal gas
2the content of S is down to 0.2g/m
3below.
6. the coke oven gas purification of vacuum carbonate desulphurization according to claim 4 and the method for recovery Sodium Thiocyanate 99, it is characterized in that: in described step 5), vaporizer adopts triple-effect evaporator, reducing by effect for maintaining its evaporator room pressure, keeping the necessary temperature difference.
7. vacuum carbonate desulphurization according to claim 6 coke oven gas purification and reclaim the method for Sodium Thiocyanate 99, it is characterized in that: a small amount of sodium sulfate of the residue after step 5) process is as fixed-end forces.
8. the coke oven gas purification of the vacuum carbonate desulphurization according to any one of claim 1 ~ 7 and the method for recovery Sodium Thiocyanate 99, is characterized in that: the water in technique is got back to previous cycles and used.
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|---|---|---|---|
| CN201410203103.8A CN104449881A (en) | 2014-05-15 | 2014-05-15 | Method for purifying coke oven gas of vacuum carbonate-process desulphurization and recovering sodium thiocyanate |
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| CN201410203103.8A CN104449881A (en) | 2014-05-15 | 2014-05-15 | Method for purifying coke oven gas of vacuum carbonate-process desulphurization and recovering sodium thiocyanate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423691A (en) * | 2018-06-07 | 2018-08-21 | 江苏燎原环保科技股份有限公司 | A method of extracting sodium sulfocyanate from HPF desulfurization waste liquors |
| CN113526471A (en) * | 2021-05-17 | 2021-10-22 | 杨想全 | Process for purifying acid gas and recovering sulfur from steel blast furnace gas and coking raw gas |
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| JP4043127B2 (en) * | 1999-02-17 | 2008-02-06 | 新日鉄エンジニアリング株式会社 | Coke oven gas purification method |
| CN101597073A (en) * | 2009-07-10 | 2009-12-09 | 重庆大学 | A kind of method for preparing Sodium Thiocyanate 99 with desulphurization waste liquid of coke oven gas |
| CN102120937A (en) * | 2010-01-07 | 2011-07-13 | 上海宝钢化工有限公司 | Purification method of coke oven gas matched with vacuum carbonate desulphurization |
| CN102336417A (en) * | 2010-07-21 | 2012-02-01 | 苏州久王多铵盐科技有限公司 | Method for recovering sodium sulfocyanate from desulfurized and decyanated wastewater of coke-oven gas |
| CN103663496A (en) * | 2013-09-24 | 2014-03-26 | 北京艾思合众环保科技有限公司 | Method for improving purity of sodium thiocyanate in coking and desulfurizing waste liquid |
-
2014
- 2014-05-15 CN CN201410203103.8A patent/CN104449881A/en active Pending
Patent Citations (5)
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| JP4043127B2 (en) * | 1999-02-17 | 2008-02-06 | 新日鉄エンジニアリング株式会社 | Coke oven gas purification method |
| CN101597073A (en) * | 2009-07-10 | 2009-12-09 | 重庆大学 | A kind of method for preparing Sodium Thiocyanate 99 with desulphurization waste liquid of coke oven gas |
| CN102120937A (en) * | 2010-01-07 | 2011-07-13 | 上海宝钢化工有限公司 | Purification method of coke oven gas matched with vacuum carbonate desulphurization |
| CN102336417A (en) * | 2010-07-21 | 2012-02-01 | 苏州久王多铵盐科技有限公司 | Method for recovering sodium sulfocyanate from desulfurized and decyanated wastewater of coke-oven gas |
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Non-Patent Citations (1)
| Title |
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| 王光辉等: ""NaSCN和Na2S2O3在水-乙醇混合"", 《武汉科技大学学报》, vol. 33, no. 4, 31 August 2010 (2010-08-31), pages 436 - 438 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423691A (en) * | 2018-06-07 | 2018-08-21 | 江苏燎原环保科技股份有限公司 | A method of extracting sodium sulfocyanate from HPF desulfurization waste liquors |
| CN113526471A (en) * | 2021-05-17 | 2021-10-22 | 杨想全 | Process for purifying acid gas and recovering sulfur from steel blast furnace gas and coking raw gas |
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Application publication date: 20150325 |