CN101428766B - Extraction of sulfur from flue gas desulfurization waste slag slurry with solvent method - Google Patents
Extraction of sulfur from flue gas desulfurization waste slag slurry with solvent method Download PDFInfo
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- CN101428766B CN101428766B CN 200810229462 CN200810229462A CN101428766B CN 101428766 B CN101428766 B CN 101428766B CN 200810229462 CN200810229462 CN 200810229462 CN 200810229462 A CN200810229462 A CN 200810229462A CN 101428766 B CN101428766 B CN 101428766B
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- sulfur
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- flue gas
- gas desulfurization
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 29
- 239000011593 sulfur Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002904 solvent Substances 0.000 title claims abstract description 26
- 239000002699 waste material Substances 0.000 title claims abstract description 21
- 239000002002 slurry Substances 0.000 title claims abstract description 17
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 16
- 230000023556 desulfurization Effects 0.000 title claims abstract description 16
- 239000003546 flue gas Substances 0.000 title claims abstract description 16
- 239000002893 slag Substances 0.000 title description 6
- 238000000605 extraction Methods 0.000 title description 5
- 239000007787 solid Substances 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 238000002386 leaching Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 13
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 claims abstract 3
- 239000000706 filtrate Substances 0.000 claims abstract 3
- 229950011008 tetrachloroethylene Drugs 0.000 claims abstract 3
- 239000000284 extract Substances 0.000 claims description 7
- 239000012452 mother liquor Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000005864 Sulphur Substances 0.000 description 20
- 238000001914 filtration Methods 0.000 description 15
- 238000002425 crystallisation Methods 0.000 description 9
- 238000001035 drying Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 101100493820 Caenorhabditis elegans best-1 gene Proteins 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 235000011194 food seasoning agent Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Treating Waste Gases (AREA)
Abstract
溶剂法从烟气脱硫废渣浆中提取硫磺，涉及一种从废渣或废浆中提取硫磺的方法，本发明公开了两种从废物中提取硫磺的方法，利用本方法可从烟气脱硫、生物处理的废渣浆中回收高品质的硫磺。将固、液混合物(或脱水、干燥成为干固体)，按照干固体、溶剂质量比1∶1～1∶15加入溶剂二硫化碳(或四氯乙烯)，在混合物温度10～45℃(四氯乙烯20～90℃)条件下，搅拌浸取5min～3h；然后，将浸取后的固液混合物保温过滤，滤液冷却结晶或蒸发结晶后过滤得固体硫磺，经低温干燥得到硫磺产品。本发明所述方法简单易行，溶剂可回收利用，并且可在较低能耗下，获得较高纯度的硫磺产品，实现了废物的合理利用。
Solvent method for extracting sulfur from flue gas desulfurization waste residue slurry relates to a method for extracting sulfur from waste residue or waste slurry. The invention discloses two methods for extracting sulfur from waste. The method can be used for flue gas desulfurization, High quality sulfur is recovered from the treated waste slurry. The solid and liquid mixture (or dehydrated and dried into a dry solid) is added to the solvent carbon disulfide (or tetrachloroethylene) according to the dry solid to solvent mass ratio of 1:1 to 1:15. (20-90°C), stirring and leaching for 5min-3h; then, heat-filter the leached solid-liquid mixture, cool and crystallize the filtrate or evaporate and crystallize to obtain solid sulfur, and dry at low temperature to obtain sulfur products. The method of the invention is simple and easy, the solvent can be recycled, and the sulfur product with higher purity can be obtained under lower energy consumption, so that the rational utilization of waste is realized.
Description
Technical field
The present invention relates to a kind of method of from waste residue or useless slurry, extracting sulphur, particularly relate to the method for extraction sulphur a kind of waste residue that after a series of processing such as flue gas desulfurization and biological treatment, obtains with solvent, the useless slurry.
Background technology
Solid, liquid mixture after flue gas desulfurization and the biological treatment generally adopt the depleted mode to handle, and do like this and have promptly wasted high-load sulphur resource wherein, have also polluted environment.Now, there is the people that this part waste residue slurry is collected, dehydration, the drying preparation sulfuric acid that burns again.Though this route can obtain sulfuric acid product, consume lot of energy.In view of the situation, the present invention adopts a kind of less energy-consumption means to obtain the novel process route of high-quality sulfur product, solves the problem of utilizing of above-mentioned waste residue slurry.
Summary of the invention
The object of the present invention is to provide that a kind of simple substance sulphur extracts the solid, liquid mixture that solvent obtains through selecting for use after flue gas desulfurization and biological treatment; And the sulfur product of acquisition higher degree; The invention discloses two kinds of methods of from refuse, extracting sulphur; Utilize present method can from the waste residue slurry of flue gas desulfurization, biological treatment, reclaim high-quality sulphur, and have advantage of low energy consumption.
The objective of the invention is to realize through following technical scheme:
Solvent method extracts sulphur from flue gas desulfurization waste slag slurry, this extraction step is: use solvent dithiocarbonic anhydride or zellon to extract wherein sulphur from flue gas desulfurization waste slag slurry according to the step of dissolving, filtration, crystallization, cryodrying.
Described solvent method extracts sulphur from flue gas desulfurization waste slag slurry, when said solvent was dithiocarbonic anhydride, its technological process was:
(1) solid material or liquid mixing raw material or dehydration, drying are become dried solid material, added dithiocarbonic anhydride than 1: 1～1: 15, under 10～46 ℃ of conditions of mixture temperature, stir leaching 5min～3h according to dried solid and solvent quality; Wherein, stir revolution 200～1500rpm;
(2) insulation of the solidliquid mixture after will leaching is filtered, and filtration cakes torrefaction reclaims dithiocarbonic anhydride, and filtrating crystallisation by cooling or evaporative crystallization after-filtration obtain solid sulfur, and filtrating gets into the mother liquor storage tank, uses when leaching next time; Solid sulfur gets sulfur product through cryodrying.
Described solvent method extracts sulphur from flue gas desulfurization waste slag slurry, when said solvent was zellon, its technological process was:
(1) solid material or liquid mixing raw material or dehydration, drying are become dried solid material, added zellon than 1: 1～1: 20, under 20～121 ℃ of conditions of mixture temperature, stir leaching 5min～3h according to dried solid and solvent quality; Wherein, stir revolution 200～1500rpm;
(2) insulation of the solidliquid mixture after will leaching is filtered, and filtration cakes torrefaction reclaims zellon, and filtrating crystallisation by cooling after-filtration obtains solid sulfur, and filtrating gets into the mother liquor storage tank, uses when leaching next time; Solid sulfur gets sulfur product through cryodrying.
Advantage of the present invention and effect are:
The method of the invention is simple, the recyclable utilization of solvent, and can obtain the sulfur product of higher degree than under the less energy-consumption, realized reasonable utilization of wastes.
Description of drawings
Accompanying drawing of the present invention is solvent method extracts sulphur from waste residue slurry a block diagram.
Embodiment
With reference to the accompanying drawings the present invention is elaborated.
The invention discloses two kinds of methods of from refuse, extracting sulphur, utilize present method can from the waste residue slurry of flue gas desulfurization, biological treatment, reclaim high-quality sulphur.
Method one: with the solid, liquid mixture that obtain after flue gas desulfurization and the biological treatment (or dehydration, drying become dried solid); (25g～375g) mass ratio added dithiocarbonic anhydride in 1: 1～1: 15 to dried solid (25g) with solvent; Under 10～46 ℃ of conditions of mixture temperature, stir leaching 5min～3h; Wherein, stir revolution 200～1500rpm; Then, the insulation of the solidliquid mixture after the leaching is filtered, filtration cakes torrefaction reclaims dithiocarbonic anhydride, and filtrating crystallisation by cooling or evaporative crystallization after-filtration obtain solid sulfur, and filtrating gets into the mother liquor storage tank, uses when leaching next time.Solid sulfur gets sulfur product through cryodrying.
Dried solid, solvent quality be than best 1: 8～1: 12, best 30～45 ℃ of leaching temperature, and the best 30min～1h of leaching time stirs the best 200～500rpm of revolution.
Method two: with the solid, liquid mixture that obtain after flue gas desulfurization and the biological treatment (or dehydration, drying become dried solid); (25g～500g) mass ratio added zellon in 1: 1～1: 20 with solvent according to dried solid (25g); Under 20～121 ℃ of conditions of mixture temperature, stir leaching 5min～3h; Wherein, stir revolution 200～1500rpm; Then, the solidliquid mixture insulation after leaching is filtered, filtration cakes torrefaction reclaims zellon, and filtrating crystallisation by cooling, filtration obtain solid sulfur, and filtrating gets into the mother liquor storage tank, uses when leaching next time, and solid sulfur gets sulfur product through cryodrying.
Solvent, dried solid masses be than best 1: 2～1: 6, best 50～90 ℃ of leaching temperature, and the best 30min～1h of leaching time stirs the best 200～500rpm of revolution.
Illustrate below:
Embodiment 1
1, dissolving (or extraction)
(1) takes by weighing the above-mentioned solid of 25g (or solidliquid mixture 62.5g of solid content 40%) and place the 500ml there-necked flask.Then, add dithiocarbonic anhydride 100ml (126g) in this there-necked flask.
(2) there-necked flask is placed the water bath with thermostatic control of 35 ℃ of water temperatures, the there-necked flask middle port is inserted the whisking appliance that has plug, mouthful insert the TM that have plug on one side, another mouthful seals with plug.
When (3) treating in the there-necked flask 35 ℃ of TM registrations, open to stir also and pick up counting, stir revolution 200rpm, behind the 30min, close stirring.
2, filtration, crystallization
(1) when dissolution process carries out, installs the filtering system of B, vacuum pump, filter flask composition, and filter paper is spread into the B bottom.
(2) open the plug of there-necked flask, the material that dissolving finishes is poured in the B rapidly.Simultaneously, the open vacuum pump when treating not drip in the liquid 60s in the B, cuts out vacuum pump.
(3) liquid in the filter flask is placed 1h in air; When treating fluid temperature near room temperature; Solidliquid mixture in the filter flask is poured in the another set of filtering system of being made up of B, vacuum pump, filter flask, solid, liquid separation are obtained the dithiocarbonic anhydride solution of wet solid of sulphur and sulphur.
(4) the dithiocarbonic anhydride evaporation, the condensing works that place electric mantle and condensing surface to form filter cake reclaim solvent wherein.
3, drying
The wet solid of sulphur is put into petridish, and put it in the ventilating kitchen, air seasoning 12 hours can obtain sulfur product.
Embodiment 2
1, dissolving (or extraction)
(1) takes by weighing the above-mentioned solid of 25g (or solidliquid mixture 62.5g of solid content 40%) and place the 500ml there-necked flask.Then, add zellon 186ml (300g) in this there-necked flask.
(2) there-necked flask is placed the water bath with thermostatic control of 70 ℃ of water temperatures, the there-necked flask middle port is inserted the whisking appliance that has plug, mouthful insert the TM that have plug on one side, another mouthful seals with plug.
When (3) treating in the there-necked flask 70 ℃ of TM registrations, open to stir also and pick up counting, stir revolution 300rpm, behind the 120min, close stirring.
2, filtration, crystallization
(1) when dissolution process carries out, installs the filtering system of B, vacuum pump, filter flask composition, and filter paper is spread into the B bottom.
(2) open the plug of there-necked flask, the material that dissolving finishes is poured in the B rapidly.Simultaneously, the open vacuum pump when treating not drip in the liquid 60s in the B, cuts out vacuum pump.
(3) liquid in the filter flask is placed 1h in air; When treating fluid temperature near room temperature; Solidliquid mixture in the filter flask is poured in the another set of filtering system of being made up of B, vacuum pump, filter flask, solid, liquid separation are obtained the zellon solution of wet solid of sulphur and sulphur.
(4) the zellon evaporation, the condensing works that place electric mantle and condensing surface to form filter cake reclaim solvent wherein.
3, drying
The wet solid of sulphur is put into petridish, and put it in the ventilating kitchen, air seasoning 12 hours can obtain sulfur product.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810229462 CN101428766B (en) | 2008-12-09 | 2008-12-09 | Extraction of sulfur from flue gas desulfurization waste slag slurry with solvent method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810229462 CN101428766B (en) | 2008-12-09 | 2008-12-09 | Extraction of sulfur from flue gas desulfurization waste slag slurry with solvent method |
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| Publication Number | Publication Date |
|---|---|
| CN101428766A CN101428766A (en) | 2009-05-13 |
| CN101428766B true CN101428766B (en) | 2012-03-21 |
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| CN 200810229462 Expired - Fee Related CN101428766B (en) | 2008-12-09 | 2008-12-09 | Extraction of sulfur from flue gas desulfurization waste slag slurry with solvent method |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977656A (en) * | 2018-08-24 | 2018-12-11 | 淄博淦达环保科技有限公司 | A kind of lixiviation process preparation process of Zinc in Zinc Concentrates and sulphur |
| CN109455674B (en) * | 2018-12-21 | 2022-04-12 | 浙江埃森化学有限公司 | Solvent purification method of ethyl chloride byproduct sulfur |
| CN109835873B (en) * | 2019-03-27 | 2020-04-24 | 淮北师范大学 | Device and method for preparing sulfur from sulfur-containing waste residues |
| CN111362231B (en) * | 2020-03-16 | 2021-06-04 | 淮北师范大学 | System and method for extracting sulfur from sulfur-containing foam in a coking plant |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1192723A (en) * | 1995-06-15 | 1998-09-09 | 法国石油公司 | Method and device for processing hydrogen sulphide-contg. gas, comprising a cooling step for crystallised sulphur removal |
-
2008
- 2008-12-09 CN CN 200810229462 patent/CN101428766B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1192723A (en) * | 1995-06-15 | 1998-09-09 | 法国石油公司 | Method and device for processing hydrogen sulphide-contg. gas, comprising a cooling step for crystallised sulphur removal |
Non-Patent Citations (2)
| Title |
|---|
| 王宁等.从硫磺废渣中回收硫磺.环境保护.1992,(6),第43页. * |
| 邱祖民等.不溶性硫磺的提纯及高温稳定性研究.南昌大学学报(理科版).2002,26(2),第103-105页. * |
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