CN102267769A - Vacuum potassium carbonate method for utilizing coke oven coal gas desulphurization and decyanation waste liquid as resource - Google Patents
Vacuum potassium carbonate method for utilizing coke oven coal gas desulphurization and decyanation waste liquid as resource Download PDFInfo
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- CN102267769A CN102267769A CN2010101917448A CN201010191744A CN102267769A CN 102267769 A CN102267769 A CN 102267769A CN 2010101917448 A CN2010101917448 A CN 2010101917448A CN 201010191744 A CN201010191744 A CN 201010191744A CN 102267769 A CN102267769 A CN 102267769A
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- prussiate
- waste liquid
- sulfide
- decyanation
- potash
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Abstract
The invention discloses a vacuum potassium carbonate method for utilizing coke oven coal gas desulphurization and decyanation waste liquid recycling as a resource. The method is also suitable to be used in other waste liquids containing high concentration cyanide and sulfide. According to the method, cyanide and sulfide are simultaneously precipitated; the precipitate is separated by centrifugation; the waste liquid processed from desulphurization and decyanation is processed through pH regulation and coagulant dosing; the processed waste liquid is discharged into a carbonization wastewater biochemical treatment system, and is treated; ferrocyanide precipitate is subject to a reaction with added lye in a high temperature, and is converted into potassium ferrocyanide; potassium ferrocyanide is disoluted, and is separated by centrifugation, such that potassium ferrocyanide mother liquor is obtained; potassium ferrocyanide mother liquor is cooled and crystallized, such that potassium ferrocyanide product is obtained. The method has advantages of simple equipment and convenient operation. With the method, simultaneous desulphurization and decyanation can be realized, requirements of subsequent treatments are satisfied, the wastes are utilized as resources, and economic benefits are brought in.
Description
Technical field
The invention belongs to changing rejected material to useful resource and process field, relate to a kind of method of vacuum salt of wormwood method coke-oven-gas desulfurization and decyanation effluent resource specifically.
Background technology
Vacuum salt of wormwood method coke-oven-gas desulfurization and decyanation technology belongs to wet absorption method sulfur removal technology.Its main technique is at first to adopt solution of potassium carbonate directly to absorb hydrogen sulfide and prussic acid in the coal gas; The rich solution that has absorbed sour gas enters regenerator column regeneration, and the water vapor that rises at the bottom of the regenerator column under vacuum and cold condition contacts, and sour gas desorbs from rich solution; The sour gas that produces can adopt Kraus process to produce elementary sulfur or adopt contact process to produce sulfuric acid.Carry out to produce the waste liquid that contains high density prussiate and sulfide in the process of coke-oven-gas desulfurization and decyanation in employing vacuum salt of wormwood method.This waste liquid mainly is made up of two portions, and wherein the part that quantity discharged is bigger is a vacuum condensation liquid, and it is to produce owing to wherein water vapor condensation when the sour gas vacuum condensation, and its main component is potassium cyanide and potassium sulphide, and is colourless, pH7～8; The less another part of quantity discharged is the salt of wormwood lean solution, it is for preventing in the salt of wormwood lean solution impurity enriched and influence prussic acid and hydrogen sulfide absorption needs a small amount of discharging that its main component is salt of wormwood, potassium cyanide and potassium sulphide, also contains organism such as tar, phenol, sorrel is about pH10.
In the coke-oven plant, usually the desulfuration and decyanation waste liquid of vacuum salt of wormwood method generation is directly to enter the coking chemical waste water biochemical treatment system to handle, but because wherein prussiate and sulfide content are all very high, up to thousands of extremely mg/L up to ten thousand, directly enter the coking chemical waste water biochemical treatment system and can produce very big restraining effect its biological activity, cause the low even paralysis of biological treatment system treatment effect, make that water outlet can not qualified discharge, this just need handle the desulfuration and decyanation waste liquid prussiate that makes wherein and sulfide and be reduced to and can enter biochemical treatment system after the level that does not influence biological treatment and further handle.Therefore developing a kind of treatment process easy, effective, easy row at this waste liquid is necessary.In addition because the content of sulfide and prussiate is very high in the desulfuration and decyanation waste liquid that vacuum salt of wormwood method produces, if in treating processes with its recycling or make other products, the expense that not only can compensation deals produces also will produce certain economic benefits.Therefore the exploitation of vacuum salt of wormwood method desulfuration and decyanation effluent resource technology not only can solve vacuum salt of wormwood method in coke oven gas purification application problem and make follow-up biochemical treatment effectively carry out, the water outlet qualified discharge has very important significance for the energy-saving and emission-reduction tool of coking industry.
At present, the resource technology of the organic liquid waste of high density prussiate that produces about vacuum salt of wormwood method and sulfide yet there are no report.But at the wastewater containing phenol and cyanide that contains low concentration prussiate and sulfide of coking industry, domestic and international research person has done a large amount of research, and has obtained certain progress.For example, the patent No. is that the contriver has mentioned a kind of electrolysis coagulation device, and fe is transformed into Fe in 200610043520.6 the Chinese patent
2+, utilize Fe
2+With the S in the wastewater containing phenol and cyanide
2-And CN
-Generate precipitation and remove the method for above two kinds of toxic substances, this method is only applicable to the processing of lower concentration prussiate and sulfide, and when concentration was high, not only power consumption was huge, and the ferroelectric utmost point is changed frequent, thereby and produce a large amount of mud and produce secondary pollution; The patent No. is that the patent of invention of CA85100375A is mentioned a kind of employing soluble ferrite and at first precipitated sulfide, the redeposition prussiate, " thick white slurry " (mixture of yellow prussiate) that will produce then removed the method that obtains the barba hispanica product behind the impurity with acid treatment, this method has its limitation for the high waste liquid of sulfide content, because prussiate and sulfide content are all higher, precipitate sulfide respectively and prussiate is had any problem by two steps, and produce that to remove the processing of the acid waste water that contains a large amount of sulfide that impurity produces also be very big problem by adding acid.The present invention proposes a kind of method and apparatus of the decyanation desulfurization waste liquor resource utilization that produces at vacuum salt of wormwood method.Promptly adopt ferrous salt that prussiate and sulfide are precipitated simultaneously, supernatant liquor enters the coking chemical waste water biochemical treatment system after by pH regulator and dosing coagulating sedimentation and handles; Precipitation adds alkali lye and makes the yellow prussiate of potash product after washing, undissolved Iron sulfuret and the new ironic hydroxide that produces also can be recycled in the filter cake.By the technology among the present invention, the waste liquid that vacuum salt of wormwood method produces not only can directly enter the coking chemical waste water biochemical treatment system after treatment, and has realized changing waste into resources, has reclaimed the yellow prussiate of potash product.
Summary of the invention
The object of the present invention is to provide a kind of method of vacuum salt of wormwood method coke-oven-gas desulfurization and decyanation effluent resource.This method adopts soluble ferrite to precipitate prussiate and sulfide simultaneously, these two kinds of toxic substances significantly is reduced to can satisfies coking chemical waste water biochemical treatment requirement, reclaims the yellow prussiate of potash product simultaneously.
Technical scheme of the present invention is as follows
At first in waste liquid, add soluble ferrite, ferrous salt and prussiate and sulfide reaction generate precipitation, then throw out is carried out centrifugation, the precipitation of ferrocyanide that obtains and the alkali lye of adding at high temperature react and change into the yellow prussiate of potash stripping, obtain the yellow prussiate of potash mother liquor through centrifugation again, crystallisation by cooling obtains the yellow prussiate of potash product then.Removing waste liquid behind sulfide and the hydride enters the coking chemical waste water biochemical treatment system after by pH regulator and dosing coagulation and handles.Specifically describe as follows.
1. sulfide and prussiate precipitate
The pH that regulates waste liquid with acid or alkali is 5～11, and controlled temperature is 20～55 ℃, adds soluble ferrite, Fe
2+With the S in the waste liquid
2-And CN
-Following principal reaction takes place:
Fe
2++S
2-→FeS↓ (1)
Fe
2++CN
-→Fe(CN)
6 4- (2)
2Fe
2+-Fe(CN)
6 4-→Fe
2Fe(CN)
6↓ (3)
3Fe
2Fe(CN)
6+O
2+4H
+→Fe
4[Fe(CN)
6]
3↓+2Fe
2++2H
2O (4)
Fe
2+With the S in the decyanation desulfurization waste liquor
2-And CN
-React and generate FeS, Fe
2Fe (CN)
6And Fe
4[Fe (CN)
6]
3Precipitation, throw out is centrifugal and liquid phase separation through whizzer.
2. yellow prussiate of potash generates
The yellow prussiate solid that centrifugation obtains enters stirred autoclave, in reactor, add concentrated base (NaOH or KOH, below be that example describes with NaOH) heating reacts, temperature of reaction is 80～160 ℃, and following reaction (is example to add NaOH) takes place in the reactor:
Fe
2Fe(CN)
6+4NaOH→Na
4Fe(CN)
6+2Fe(OH)
2↓ (5)
Fe
4[Fe(CN)
6]
3+12NaOH→3Na
4Fe(CN)
6+4Fe(OH)
3↓ (6)
High alkali liquid and Fe
2Fe (CN)
6, and Fe
4[Fe (CN)
6]
3Reaction generates yellow prussiate of potash (Na
4Fe (CN)
6) solution and Fe (OH)
2, Fe (OH)
3Precipitation.Fe (OH)
2, Fe (OH)
3The FeS that reaction generates with previous step is by centrifugal and yellow prussiate of potash solution separating.
3. yellow prussiate of potash product crystallization
The yellow prussiate of potash mother liquor of heat enters crystallizer tank, and after cooling under 5～25 ℃, the yellow prussiate of potash crystallization is separated out, and crystallized product obtains the yellow prussiate of potash product by centrifugation.Can get back to the stirred autoclave recycle with the residue alkali lye of centrifugal generation after the crystallization, add fresh alkali lye simultaneously to satisfy the requirement of products production.
4. wastewater treatment
Remove waste liquid behind sulfide and the hydride by pH regulator with add and enter coking wastewater processing system after coagulating agent is removed the solid matter coagulating sedimentation and handle.
Device and the equipment of realizing the desulfuration and decyanation effluent resource mainly comprise: the required heatable stirred autoclave of precipitin reaction that is used for ferrous salt and prussiate, sulfide, the whizzer that is used for precipitation separation, be used for alkali lye and precipitation generate the yellow prussiate of potash reaction required heat stirred autoclave, be used for the isolating whizzer of yellow prussiate of potash mother liquor, be used for the crystallizer tank and the whizzer that is used for the yellow prussiate of potash Crystallization Separation of yellow prussiate of potash mother liquor crystallization.
Description of drawings
Accompanying drawing is vacuum salt of wormwood method desulfuration and decyanation effluent resource system device of the present invention and process flow sheet.Among the figure: 1---stirred autoclave 1; 2---whizzer 1; 3---stirred autoclave 2; 4---whizzer 2; 5---crystallizer tank; 6---whizzer 3; 7---the pH regulator groove; 8---coagulation tank; 9---vertical sedimentation basin.
Embodiment
Below in conjunction with accompanying drawing principle of the present invention, equipment and technical process are further described.As shown in the figure, the desulfuration and decyanation waste liquid at first enters stirred autoclave 1, adding ferrous salt in reactor 1 precipitates prussiate and sulfide simultaneously, liquid-solid mixture enters whizzer 1 and carries out centrifugation then, wherein liquid phase enters the coking chemical waste water biochemical treatment system after by pH regulator and dosing coagulating sedimentation and handles, solid phase enters stirred autoclave 2, and the yellow prussiate wherein and the alkali lye of adding (NaOH or KOH) reaction generates Fe (OH)
2The yellow prussiate of potash of precipitation and solubilised state.Enter whizzer 2 then and carry out centrifugation, the yellow prussiate of potash mother liquor enters the crystallizer tank cooling again and obtains the yellow prussiate of potash crystallization, the yellow prussiate of potash crystallisate enters whizzer 3 and dewaters and obtain the yellow prussiate of potash product, and undissolved Iron sulfuret and the new ironic hydroxide that produces also can carry out reuse in the filter cake.The residue alkali lye that crystallizer tank and whizzer 3 produce can be got back to stirred autoclave 2 and carry out recycle, replenishes fresh alkali lye simultaneously to satisfy reaction needed. Reactor 1,2 is by the steam heating control reaction temperature.
Below enumerate embodiment effect of the present invention is described, but claim scope of the present invention is not limited only to this.
Embodiment 1: vacuum salt of wormwood method desulfuration and decyanation liquid waste disposal lab scale, and every batch processed amount 1L, former waste liquid total cyanide concentration is 14853mg/L, S
2-Be 4519mg/L.React through adding ferrous sulfate, 50 ℃ of temperature, pH is 6, the about 738mg/L of water outlet prussiate, S
2-Less than 25mg/L, clearance adds NaOH all greater than 95% behind the sedimentation and filtration, and 90 ℃ of reactions generate yellow prussiate of potash, 15 ℃ of crystallizations, and every liter of waste water reclaims yellow prussiate of potash 26g approximately.
Embodiment 2: vacuum salt of wormwood method desulfuration and decyanation liquid waste disposal lab scale, and every batch processed amount 1L, former waste liquid total cyanide concentration is 10704mg/L, S
2-Be 3120mg/L.React through adding ferrous sulfate, 50 ℃ of temperature, pH is 6, the about 500mg/L of water outlet prussiate, S
2-Less than 15mg/L, clearance adds NaOH all greater than 95% behind the sedimentation and filtration, and 90 ℃ of reactions generate yellow prussiate of potash, 15 ℃ of crystallizations, and every liter of waste water reclaims yellow prussiate of potash 18g approximately.
Embodiment 3: vacuum salt of wormwood method desulfuration and decyanation liquid waste disposal lab scale, and every batch processed amount 1L, former waste liquid total cyanide concentration is 655mg/L, S
2-Be 306mg/L.React through adding iron protochloride, 30 ℃ of temperature, pH is 7, the about 30mg/L of water outlet prussiate, S
2-Less than 1.5mg/L, clearance adds KOH all greater than 95% behind the sedimentation and filtration, and 95 ℃ of reactions generate yellow prussiate of potash, 20 ℃ of crystallizations, and every liter of waste water reclaims yellow prussiate of potash 1.4g approximately.
Claims (4)
1. vacuum salt of wormwood method coke-oven-gas desulfurization and decyanation effluent resource method, it is characterized in that: at first in the desulfuration and decyanation waste liquid, add soluble ferrite and precipitate prussiate and sulfide in the waste liquid simultaneously, throw out at high temperature reacts under 80～160 ℃ of conditions with dense sodium hydroxide or potassium hydroxide alkali lye after centrifugation goes out and generates yellow prussiate of potash, the yellow prussiate of potash mother liquor is at 5～25 ℃ of following crystallisation by cooling, crystallisate obtains the yellow prussiate of potash product through centrifugation, the alkali lye reusable edible; The waste liquid that removes behind most of prussiate and the sulfide can directly enter coking chemical waste water conventional processing system behind pH regulator and coagulating sedimentation.
2. method according to claim 1 is characterized in that waste liquid is the sulfur compound that produces in the vacuum salt of wormwood method coke-oven-gas desulfurization and decyanation process and the waste liquid of prussiate; Contained prussiate is simple prussiate in the waste liquid, but not network and prussiate; The concentration of prussiate is 500～15000mg/L, and sulfide concentration is 0～10000mg/L; Be applicable to that also other contain the waste liquid of high density sulfide and prussiate.
3. method according to claim 1 is characterized in that soluble ferrite is ferrous sulfate, iron protochloride.
4. method according to claim 1 is characterized in that adopting the temperature of reaction of ferrous salt precipitation sulfide and prussiate is 20～55 ℃, and pH is 5～11.
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|---|---|---|---|
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|---|---|---|---|
| CN 201010191744 CN102267769B (en) | 2010-06-04 | 2010-06-04 | Vacuum potassium carbonate method for utilizing coke oven coal gas desulphurization and decyanation waste liquid as resource |
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|---|---|
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| CN102267769B CN102267769B (en) | 2013-10-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351891A (en) * | 2013-05-07 | 2013-10-16 | 程相魁 | New process for carrying out desulfurization, decyanation and decarbonization by using sodium hydroxide and separating reaction products |
| CN103395910A (en) * | 2013-07-26 | 2013-11-20 | 北京赛科康仑环保科技有限公司 | Vacuum potassium carbonate desulfurization liquid waste treatment technology and device |
| CN104071884A (en) * | 2013-03-29 | 2014-10-01 | 上海宝钢化工有限公司 | Vacuum potassium carbonate desulfurizing solution post processing method |
| CN104609645A (en) * | 2014-12-17 | 2015-05-13 | 武汉钢铁(集团)公司 | Coking vacuum potash desulfurization waste solution desulfurization and decyanation pretreatment method and device |
| CN104946315A (en) * | 2014-03-31 | 2015-09-30 | 江苏联峰能源装备有限公司 | Method for purifying coke oven gas and recycling desulfurated liquid waste by virtue of vacuum potassium carbonate method |
| CN105003826A (en) * | 2015-07-02 | 2015-10-28 | 广东韶钢松山股份有限公司 | Annular pipe network for acid steam conveying |
| CN105130097A (en) * | 2015-07-22 | 2015-12-09 | 武汉科技大学 | Treatment method of vacuum potassium carbonate method coke oven gas desulfurization waste liquid |
| CN105130099A (en) * | 2015-07-24 | 2015-12-09 | 武汉科技大学 | Method of treating vacuum potassium carbonate desulfurization waste liquid through acidic separation-out/oxidization process |
| CN105776675A (en) * | 2016-05-31 | 2016-07-20 | 武汉钢铁股份有限公司 | Device and method for desulfuration and decyanation treatment of waste liquid generated in vacuum potassium carbonate desulfurization process |
| CN105836972A (en) * | 2016-05-20 | 2016-08-10 | 武汉钢铁股份有限公司 | Treatment method and system of wastewater |
| CN106147884A (en) * | 2015-03-28 | 2016-11-23 | 鞍钢股份有限公司 | Cyanogen process and device drop in a kind of novel gas desulfurization and waste water |
| CN107758817A (en) * | 2017-09-12 | 2018-03-06 | 河钢股份有限公司邯郸分公司 | A kind of high-efficiency desulfurization decyanation medicament |
| CN111675388A (en) * | 2020-07-13 | 2020-09-18 | 德州金智环保科技有限公司 | Synchronous desulfurization and decyanation method and device for coal chemical gas-making sewage |
| CN113105012A (en) * | 2020-01-13 | 2021-07-13 | 中国科学院过程工程研究所 | Treatment device and method for desulfurization and decyanation waste liquid in coal chemical industry |
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-
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Patent Citations (3)
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| CN85100375A (en) * | 1985-04-01 | 1986-09-03 | 湘潭钢铁厂 | Cyan-containing waste water treatment by iron blue method |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104071884A (en) * | 2013-03-29 | 2014-10-01 | 上海宝钢化工有限公司 | Vacuum potassium carbonate desulfurizing solution post processing method |
| CN103351891B (en) * | 2013-05-07 | 2015-04-29 | 程相魁 | New process for carrying out desulfurization, decyanation and decarbonization by using sodium hydroxide and separating reaction products |
| CN103351891A (en) * | 2013-05-07 | 2013-10-16 | 程相魁 | New process for carrying out desulfurization, decyanation and decarbonization by using sodium hydroxide and separating reaction products |
| CN103395910B (en) * | 2013-07-26 | 2016-01-27 | 北京赛科康仑环保科技有限公司 | A kind of Vacuum potassium carbonate desulfurization liquid waste treatment technology and device |
| CN103395910A (en) * | 2013-07-26 | 2013-11-20 | 北京赛科康仑环保科技有限公司 | Vacuum potassium carbonate desulfurization liquid waste treatment technology and device |
| CN104946315A (en) * | 2014-03-31 | 2015-09-30 | 江苏联峰能源装备有限公司 | Method for purifying coke oven gas and recycling desulfurated liquid waste by virtue of vacuum potassium carbonate method |
| CN104609645A (en) * | 2014-12-17 | 2015-05-13 | 武汉钢铁(集团)公司 | Coking vacuum potash desulfurization waste solution desulfurization and decyanation pretreatment method and device |
| CN106147884A (en) * | 2015-03-28 | 2016-11-23 | 鞍钢股份有限公司 | Cyanogen process and device drop in a kind of novel gas desulfurization and waste water |
| CN105003826A (en) * | 2015-07-02 | 2015-10-28 | 广东韶钢松山股份有限公司 | Annular pipe network for acid steam conveying |
| CN105130097A (en) * | 2015-07-22 | 2015-12-09 | 武汉科技大学 | Treatment method of vacuum potassium carbonate method coke oven gas desulfurization waste liquid |
| CN105130099A (en) * | 2015-07-24 | 2015-12-09 | 武汉科技大学 | Method of treating vacuum potassium carbonate desulfurization waste liquid through acidic separation-out/oxidization process |
| CN105836972A (en) * | 2016-05-20 | 2016-08-10 | 武汉钢铁股份有限公司 | Treatment method and system of wastewater |
| CN105776675A (en) * | 2016-05-31 | 2016-07-20 | 武汉钢铁股份有限公司 | Device and method for desulfuration and decyanation treatment of waste liquid generated in vacuum potassium carbonate desulfurization process |
| CN107758817A (en) * | 2017-09-12 | 2018-03-06 | 河钢股份有限公司邯郸分公司 | A kind of high-efficiency desulfurization decyanation medicament |
| CN113105012A (en) * | 2020-01-13 | 2021-07-13 | 中国科学院过程工程研究所 | Treatment device and method for desulfurization and decyanation waste liquid in coal chemical industry |
| CN111675388A (en) * | 2020-07-13 | 2020-09-18 | 德州金智环保科技有限公司 | Synchronous desulfurization and decyanation method and device for coal chemical gas-making sewage |
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