CN103395805B - The method of high-quality Sodium Thiocyanate 99 is prepared with coke-oven-gas desulfurization and decyanation waste liquid - Google Patents
The method of high-quality Sodium Thiocyanate 99 is prepared with coke-oven-gas desulfurization and decyanation waste liquid Download PDFInfo
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- CN103395805B CN103395805B CN201310301170.9A CN201310301170A CN103395805B CN 103395805 B CN103395805 B CN 103395805B CN 201310301170 A CN201310301170 A CN 201310301170A CN 103395805 B CN103395805 B CN 103395805B
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- sodium thiocyanate
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- 239000002699 waste material Substances 0.000 title claims abstract description 26
- 239000007788 liquid Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 21
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 title claims abstract description 16
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 14
- 230000023556 desulfurization Effects 0.000 title claims abstract description 12
- 238000007255 decyanation reaction Methods 0.000 title claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 8
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 4
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 abstract description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001085 differential centrifugation Methods 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 2
- 239000010808 liquid waste Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- Treating Waste Gases (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of method preparing high-quality Sodium Thiocyanate 99 with coke-oven-gas desulfurization and decyanation waste liquid, desulfuration and decyanation waste liquid is through activated carbon decolorizing, after filtration, in waste liquid, auxiliary agent A is added under stirring, Specific amounts is the 50%-200% of Sulfothiorine molal quantity in waste liquid, thiosulfuric acid sodium ion in removing waste liquid system, cross afterwards and filter insoluble substance, backward filtrate in add a small amount of auxiliary agent C regulate pH be 5-10, distillation and concentration removes moisture afterwards, utilize differing temps, under concentration, the differential centrifugation of various Solubility of Substances isolates inorganic salt impurities, after through activated carbon decolorizing, reconcentration crystallization output finished product Sodium Thiocyanate 99.Present invention process is simple, and with low cost, the weight content of the potassium sulfocyanate of output is more than 99%.
Description
Technical field
The present invention relates to a kind of method preparing high-quality Sodium Thiocyanate 99 with coke-oven-gas desulfurization and decyanation waste liquid, belong to chemical technology field.
Background technology
" Coal Chemical Industry " magazine 01 phase in 2011, publish by " the coke-oven gas HPF sulfur removal technology liquid waste disposal new technology " of the works such as Liu Chenming, Wang Bo, Cao Hongbin, Sheng Yuxing, Li Yuping, Lin Xiao, Zhang Yi civilian, sketch HPF desulfurization process, and analyze its relative merits; Compared for the treatment process of several frequently seen desulfurization waste liquor, and highlight a kind of HPF sulfur removal technology liquid waste disposal new technology relating to multiple processes such as reaction, separation.
This technology achieves 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 longer, investment is higher, promote difficulty larger.
With sodium (sodium carbonate, sodium hydroxide) for the desulfurizing and decyanating method for coke oven gas of alkali source has: tannin process, A.D.A method, improvement A.D.A method, PDS method, PDS+ tannin process etc.
Waste liquid index is (by weight): Sodium Thiocyanate 99: about 5%-25%; Sodium sulfate: 1%-10%; Sulfothiorine: 0.1%-15%; Sodium carbonate and other material a small amount of.
How to be applied by this waste liquid, be a new research topic.
Summary of the invention
The technical issues that need to address of the present invention are just the defect overcoming prior art, provide a kind of method preparing high-quality Sodium Thiocyanate 99 with coke-oven-gas desulfurization and decyanation waste liquid, and its technique is simple, and with low cost, the weight content of the potassium sulfocyanate of output is more than 99%.
For solving the problem, the present invention adopts following technical scheme:
The invention provides a kind of method preparing high-quality Sodium Thiocyanate 99 with coke-oven-gas desulfurization and decyanation waste liquid, described method is:
Desulfuration and decyanation waste liquid is after activated carbon decolorizing, filtration, in waste liquid, auxiliary agent A is added under stirring, Specific amounts is the 50%-200% of Sulfothiorine molal quantity in waste liquid, thiosulfuric acid sodium ion in removing waste liquid system, cross afterwards and filter insoluble substance, backward filtrate in add a small amount of auxiliary agent C regulate pH be 5-10, distillation and concentration removes moisture afterwards, under utilizing differing temps, concentration, the differential centrifugation of various Solubility of Substances isolates inorganic salt impurities, after 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, the described material that can react with Sulfothiorine is oxygenant, acidic substance and prussiate etc., 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 Specific amounts of auxiliary agent A of the present invention is the 90%-110% of Sulfothiorine molal quantity in waste liquid, and auxiliary agent C adjusts pH to be 6-8.
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.
Present invention process is simple, and with low cost, the weight content of the potassium sulfocyanate of output is more than 99%.
Embodiment
It is (by weight) with the coke-oven-gas desulfurization and decyanation waste liquid index that sodium (sodium carbonate, sodium hydroxide) is alkali source: Sodium Thiocyanate 99: about 5%-25%; Sodium sulfate: 1%-10%; Sulfothiorine: 0.1%-15%; Sodium carbonate and other material a small amount of.
Get waste liquid 1000g, Sodium Thiocyanate 99: about 15% sodium sulfate: 5% Sulfothiorine: 7%, sodium carbonate is a small amount of.
First in waste liquid, auxiliary agent A Sodium Persulfate 72 grams is added, stir 30 minutes, filter afterwards and remove solid impurity, in filtrate, add 3 grams of auxiliary agent C sodium hydroxide adjust ph is 6.5, 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 the described material that can react with Sulfothiorine is oxygenant, acidic substance and prussiate etc., 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.
Last it is noted that obviously, above-described embodiment is only for example of the present invention is clearly described, and the restriction not 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 exhaustive without the need to also giving all embodiments.And thus the apparent change of amplifying out or variation be still among protection scope of the present invention.
Claims (1)
1. prepare a method for high-quality Sodium Thiocyanate 99 with coke-oven-gas desulfurization and decyanation waste liquid, it is characterized in that, described method is:
Taking sodium as the coke-oven-gas desulfurization and decyanation waste liquid index of alkali source is by weight, Sodium Thiocyanate 99 5%-25%; Sodium sulfate 1%-10%; Sulfothiorine 0.1%-15%; Sodium carbonate and other material a small amount of;
Get waste liquid 1000g, Sodium Thiocyanate 99 15%; Sodium sulfate 5% Sulfothiorine 7%, sodium carbonate is a small amount of;
First in waste liquid, auxiliary agent A Sodium Persulfate 72 grams is added, stir 30 minutes, filter afterwards and remove solid impurity, in filtrate, add 3 grams of auxiliary agent C sodium hydroxide adjust ph is 6.5, filtrate concentrates afterwards, after crystallisation by cooling, centrifugation goes out sodium sulfate, and system finally obtains product Sodium Thiocyanate 99 through activated carbon decolorizing, crystallization afterwards;
Wherein, centrifuge mother liquor can circulate concentrated.
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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 true CN103395805B (en) | 2016-03-30 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115634474A (en) * | 2022-11-08 | 2023-01-24 | 鞍山市利多环保科技有限公司 | Low-temperature aeration separation method applied to two saturated inorganic sodium salt solutions |
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 desulfurization 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 desulfurization and decyanation wastewater |
Non-Patent Citations (1)
| Title |
|---|
| 焦化脱硫废液回收副盐转化的探讨;徐刚等;《第十四届冶金反应工程学学术会议论文集》;20110728;第1-6页 * |
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Application publication date: 20131120 Assignee: Wuhai Lvbang Environmental Protection Technology Co.,Ltd. Assignor: JIANGSU LIAOYUAN ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Contract record no.: X2023150000002 Denomination of invention: Method for preparing high-quality sodium thiocyanate from coke oven gas desulfurization and decyanation waste liquid Granted publication date: 20160330 License type: Common License Record date: 20230517 |