CN103395805A - Method for preparing high-quality sodium thiocyanate from desulfurized and decyanated waste liquid of coke oven gas - Google Patents
Method for preparing high-quality sodium thiocyanate from desulfurized and decyanated waste liquid of coke oven gas Download PDFInfo
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- CN103395805A CN103395805A CN2013103011709A CN201310301170A CN103395805A CN 103395805 A CN103395805 A CN 103395805A CN 2013103011709 A CN2013103011709 A CN 2013103011709A CN 201310301170 A CN201310301170 A CN 201310301170A CN 103395805 A CN103395805 A CN 103395805A
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Abstract
The invention discloses a method for preparing high-quality sodium thiocyanate from a desulfurized and decyanated waste liquid of coke oven gas, which comprises the following steps: decolorizing and filtering the desulfurized and decyanated waste liquid through activated carbon, and adding an assistant A into the waste liquid while stirring, wherein the specific quantity of the assistant A is 50-200% of the molal quantity of sodium thiosulfate in the waste liquid; removing sodium thiosulfate ions in the waste liquid system, filtering to remove insoluble substances, and then adding a small quantity of assistant C into the filtrate to regulate the pH value to 5-10; distilling and concentrating to remove the moisture, and centrifuging to separate out inorganic salt impurities based on the difference of various substances in solubility under different temperatures and concentrations; and decolorizing through activated carbon, and further concentrating and crystallizing to produce the sodium thiocyanate finished product. According to the invention, the process is simple, the cost is low, and the weight content of the produced potassium thiocyanate is more than 99%.
Description
Technical field
The present invention relates to a kind of method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid, belong to chemical technology field.
Background technology
" Coal Chemical Industry " magazine 01 phase in 2011, published " the coke-oven gas HPF sulfur removal technology liquid waste disposal new technology " literary composition by works such as Liu Chenming, Wang Bo, Cao Hongbin, Sheng Yuxing, Li Yuping, woods dawn, Zhang Yi, sketch the HPF desulfurization process, and analyzed its relative merits; Contrast the treatment process of several frequently seen desulfurization waste liquor, and highlighted a kind of HPF sulfur removal technology liquid waste disposal new technology that relates to a plurality of processes such as reaction, separation.
This technology has realized the desulfurization waste liquor resource utilization, and has the advantages such as processing efficiency is high, product purity is high, equipment mature and reliable, has good Technical Economy and application prospect.
But this technical matters is long, investment is higher, promotes difficulty larger.
Desulfurizing and decyanating method for coke oven gas take sodium (sodium carbonate, sodium hydroxide) as alkali source has: tannin extract method, A.D.A method, improvement A.D.A method, PDS method, PDS+ tannin extract method etc.
The waste liquid index is (by weight): Sodium Thiocyanate 99: 5%-25% left and right; Sodium sulfate: 1%-10%; Sulfothiorine: 0.1%-15%; Sodium carbonate and other material are a small amount of.
How this waste liquid being applied, is a new research topic.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defect of prior art, and a kind of method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid is provided, and its technique is simple, and is with low cost, and the weight content of the potassium sulfocyanate of output is more than 99%.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid, described method is:
The desulfuration and decyanation waste liquid is after activated carbon decolorizing, filtration, add auxiliary agent A under stirring in waste liquid, concrete amount is the 50%-200% of Sulfothiorine molal quantity in waste liquid, remove the thiosulfuric acid sodium ion in the waste liquid system, remove by filter afterwards insoluble substance, be 5-10 to adding in filtrate a small amount of auxiliary agent C to regulate pH afterwards, distillation and concentration removes moisture afterwards, utilize the differential centrifugation of various Solubility of Substances under differing temps, concentration to isolate inorganic salt impurity, afterwards through activated carbon decolorizing, reconcentration crystallization output finished product Sodium Thiocyanate 99.
Auxiliary agent A of the present invention is a kind of material that can react with Sulfothiorine, described can be oxygenant, acidic substance and prussiate etc. with the material of Sulfothiorine reaction, described auxiliary agent C is a kind of inorganics, and described inorganics is mineral acid, mineral alkali or inorganic salt.
Preferably, concentrated mother liquor recycle of the present invention.
Further preferably, the concrete amount of auxiliary agent A of the present invention is the 90%-110% of Sulfothiorine molal quantity in waste liquid, and it is 6-8 that auxiliary agent C transfers pH.
Further preferably, auxiliary agent A of the present invention is Sodium Persulfate, sulfuric acid, oxygen or sodium cyanide; Auxiliary agent C is sodium hydroxide, ammoniacal liquor or sulfuric acid.
Technique of the present invention is simple, and is with low cost, and the weight content of the potassium sulfocyanate of output is more than 99%.
Embodiment
Coke-oven-gas desulfurization and decyanation waste liquid index take sodium (sodium carbonate, sodium hydroxide) as alkali source is as (by weight): Sodium Thiocyanate 99: 5%-25% left and right; Sodium sulfate: 1%-10%; Sulfothiorine: 0.1%-15%; Sodium carbonate and other material are a small amount of.
Get waste liquid 1000g, Sodium Thiocyanate 99: 15% left and right sodium sulfate: 5% Sulfothiorine: 7%, sodium carbonate is a small amount of.
At first add auxiliary agent A Sodium Persulfate 72 grams in waste liquid, stirred 30 minutes, filter afterwards and remove solid impurity, be 6.5 to adding in filtrate 3 gram auxiliary agent C sodium hydroxide to regulate the pH values, filtrate concentrates afterwards, after crystallisation by cooling, centrifugation goes out sodium sulfate, and system finally obtains product Sodium Thiocyanate 99 82 grams through activated carbon decolorizing, crystallization afterwards.The weight content of the potassium sulfocyanate of output is more than 99%.
Centrifuge mother liquor can circulate concentrated.
In the present embodiment, described auxiliary agent A is a kind of material that can react with Sulfothiorine, and described can be oxygenant, acidic substance and prussiate etc. with the material of Sulfothiorine reaction, as Sodium Persulfate, sulfuric acid, oxygen or sodium cyanide etc.; Described auxiliary agent C is a kind of inorganics, and described inorganics is mineral acid, mineral alkali or inorganic salt, as: sodium hydroxide, ammoniacal liquor, sulfuric acid.
It should be noted that finally: obviously, above-described embodiment is only for example of the present invention clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (5)
1. a method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid, is characterized in that, described method is:
The desulfuration and decyanation waste liquid is after activated carbon decolorizing, filtration, add auxiliary agent A under stirring in waste liquid, concrete amount is the 50%-200% of Sulfothiorine molal quantity in waste liquid, remove the thiosulfuric acid sodium ion in the waste liquid system, remove by filter afterwards insoluble substance, be 5-10 to adding in filtrate a small amount of auxiliary agent C to regulate pH afterwards, distillation and concentration removes moisture afterwards, utilize the differential centrifugation of various Solubility of Substances under differing temps, concentration to isolate inorganic salt impurity, afterwards through activated carbon decolorizing, reconcentration crystallization output finished product Sodium Thiocyanate 99.
2. the method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid as claimed in claim 1, it is characterized in that, described auxiliary agent A is a kind of material that can react with Sulfothiorine, described can be oxygenant, acidic substance and prussiate etc. with the material of Sulfothiorine reaction, described auxiliary agent C is a kind of inorganics, described inorganics is mineral acid, mineral alkali or inorganic salt.
3. the method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid as claimed in claim 2, is characterized in that, described concentrated mother liquor recycle.
4., as the arbitrary described method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid of claim 1-3, it is characterized in that, the concrete amount of auxiliary agent A is the 90%-110% of Sulfothiorine molal quantity in waste liquid, and it is 6-8 that auxiliary agent C transfers pH.
5. the method for preparing high-quality Sodium Thiocyanate 99 with the coke-oven-gas desulfurization and decyanation waste liquid as claimed in claim 4, is characterized in that, auxiliary agent A is Sodium Persulfate, sulfuric acid, oxygen or sodium cyanide; Auxiliary agent C is sodium hydroxide, ammoniacal liquor or sulfuric acid.
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| CN201310301170.9A CN103395805B (en) | 2013-07-18 | 2013-07-18 | The method of high-quality Sodium Thiocyanate 99 is prepared with coke-oven-gas desulfurization and decyanation waste liquid |
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| CN201310301170.9A CN103395805B (en) | 2013-07-18 | 2013-07-18 | The method of high-quality Sodium Thiocyanate 99 is prepared with coke-oven-gas desulfurization and decyanation waste liquid |
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| CN103395805B CN103395805B (en) | 2016-03-30 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601219A (en) * | 2013-11-27 | 2014-02-26 | 安徽工业大学 | Method for extracting sodium carbonate and sodium thiocyanate from sodium alkali desulfurization liquid waste by using causticization-acidification method |
| CN104071915A (en) * | 2014-03-31 | 2014-10-01 | 河北九天医药化工有限公司 | Method for purifying sodium thiocyanate mother liquid through chemical reaction process |
| CN105800649A (en) * | 2016-03-09 | 2016-07-27 | 北京富海天环保科技有限公司 | Method for preparing sodium thiocyanate from ammonia desulphurization waste liquid and sodium carbonate as raw material |
| CN107651793A (en) * | 2016-07-26 | 2018-02-02 | 重庆大学 | A kind of chlorohydric acid pickling Waste Water Treatment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03257014A (en) * | 1990-03-02 | 1991-11-15 | Kansai Coke & Chem Co Ltd | Production of high purity rhodan salt |
| CN102259896A (en) * | 2011-06-21 | 2011-11-30 | 安徽工业大学 | Method for extracting sodium thiocyanate from coking desulfurization waste liquid |
| 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 |
| CN102424401A (en) * | 2011-08-22 | 2012-04-25 | 宜兴市燎原化工有限公司 | Method for recovering thiocyanate from coke oven gas desulfuration and decyanation wastewater |
-
2013
- 2013-07-18 CN CN201310301170.9A patent/CN103395805B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03257014A (en) * | 1990-03-02 | 1991-11-15 | Kansai Coke & Chem Co Ltd | Production of high purity rhodan salt |
| 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 |
| CN102259896A (en) * | 2011-06-21 | 2011-11-30 | 安徽工业大学 | Method for extracting sodium thiocyanate from coking desulfurization waste liquid |
| CN102424401A (en) * | 2011-08-22 | 2012-04-25 | 宜兴市燎原化工有限公司 | Method for recovering thiocyanate from coke oven gas desulfuration and decyanation wastewater |
Non-Patent Citations (1)
| Title |
|---|
| 徐刚等: "焦化脱硫废液回收副盐转化的探讨", 《第十四届冶金反应工程学学术会议论文集》, 28 July 2011 (2011-07-28) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601219A (en) * | 2013-11-27 | 2014-02-26 | 安徽工业大学 | Method for extracting sodium carbonate and sodium thiocyanate from sodium alkali desulfurization liquid waste by using causticization-acidification method |
| CN103601219B (en) * | 2013-11-27 | 2015-12-09 | 安徽工业大学 | From sodium alkali desulfurization waste liquor, the method for sodium carbonate and Sodium Thiocyanate 99 is extracted with causticization-acidization |
| CN104071915A (en) * | 2014-03-31 | 2014-10-01 | 河北九天医药化工有限公司 | Method for purifying sodium thiocyanate mother liquid through chemical reaction process |
| CN105800649A (en) * | 2016-03-09 | 2016-07-27 | 北京富海天环保科技有限公司 | Method for preparing sodium thiocyanate from ammonia desulphurization waste liquid and sodium carbonate as raw material |
| CN107651793A (en) * | 2016-07-26 | 2018-02-02 | 重庆大学 | A kind of chlorohydric acid pickling Waste Water Treatment |
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| CN103395805B (en) | 2016-03-30 |
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