CN1587047A - Recovery method for potassium chloride from waste tail liquid by carnallite flotation process - Google Patents
Recovery method for potassium chloride from waste tail liquid by carnallite flotation process Download PDFInfo
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- CN1587047A CN1587047A CN 200410073691 CN200410073691A CN1587047A CN 1587047 A CN1587047 A CN 1587047A CN 200410073691 CN200410073691 CN 200410073691 CN 200410073691 A CN200410073691 A CN 200410073691A CN 1587047 A CN1587047 A CN 1587047A
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- Prior art keywords
- solution
- repone
- caking agent
- pond
- alpha
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 title claims abstract description 13
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 11
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 11
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 title claims abstract description 9
- 239000002699 waste material Substances 0.000 title claims abstract description 9
- 238000011084 recovery Methods 0.000 title claims description 10
- 238000005188 flotation Methods 0.000 title abstract 2
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000004744 fabric Substances 0.000 claims description 16
- 239000004800 polyvinyl chloride Substances 0.000 claims description 16
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 16
- IJVRPNIWWODHHA-UHFFFAOYSA-N 2-cyanoprop-2-enoic acid Chemical compound OC(=O)C(=C)C#N IJVRPNIWWODHHA-UHFFFAOYSA-N 0.000 claims description 12
- 229920003023 plastic Polymers 0.000 claims description 12
- 239000004033 plastic Substances 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 6
- 240000006909 Tilia x europaea Species 0.000 claims description 6
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 6
- 239000004571 lime Substances 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000010276 construction Methods 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 230000003760 hair shine Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 238000005352 clarification Methods 0.000 claims description 2
- 239000013505 freshwater Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000013311 vegetables Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 229910001508 alkali metal halide Inorganic materials 0.000 abstract description 2
- 150000008045 alkali metal halides Chemical class 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 229910052736 halogen Inorganic materials 0.000 description 8
- 150000002367 halogens Chemical class 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 241001131796 Botaurus stellaris Species 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The present invention belongs to the field of alkali metal halide producing technology, and aims at recovering tail liquid in low cost and high recovering rate. The process of recovering potassium chloride from waste tail liquid of carnallite flotation process includes the steps of sunning tail salt solution, spreading to sun, storing, cooling to separate, dissolving coarse potassium chloride and crystallization, and refining potassium chloride crystal. The present invention has the advantages of utilizing waste tail liquid, no environmental pollution, high recovering rate, low production cost, etc.
Description
Technical field
The present invention relates to the alkali metal halide technical field, specifically a kind of preparation method of Repone K.
Background technology
Repone K is the principal item of agriculture potash fertilizer, also is the industrial main raw material of producing other sylvite.The Repone K manufacturing enterprise of China 70% continues to use traditional carnallite floatation technology at present, 1 ton of Repone K of the every production of this technology, must discharge about 8 tons waste water, usual 30,000 tons of Repone K output must be discharged 240,000 tons of waste water, have only small part enterprise to adopt adding halogen method that waste water is tedded E point and F point to the phasor respectively, convert halogen with the bittern that E selects and F selects in converting the halogen device and separate out low-sodium carnalite, low-sodium carnalite gets finished product through the secondary washing drying and packaging.Adding halogen method needs a large amount of E halogen and F halogen, and the investment of founding the factory is big, and the rate of recovery is low.
Summary of the invention
The present invention is for the problem that investment is big, the rate of recovery is low of founding the factory that overcomes in the prior art a large amount of tail washings and go out of use and adding halogen method exists, and proposes a kind of recovery method that utilizes Repone K in depleted tail washings, free from environmental pollution, the rate of recovery is high, production cost the is low carnallite floatation method waste tail liquid.
Concrete technical scheme is as follows:
The recovery method of Repone K in the carnallite floatation method waste tail liquid may further comprise the steps:
(1) tail salt solution shines in advance: tail salt solution is shone in advance, and precipitated sodium chloride when shining when concentration is 29Be, separates obtaining sodium-chlor and solution 1;
(2) ted solution 1: solution 1 is continued to ted, separate out low-grade carnallitite, shine to mother liquid concentration and reach 31.2～31.5Be, separate obtaining solution 2;
(3) store: solution 2 is avoided evaporatively being stored in the groove;
(4) freezing, separation: when temperature is reduced to below-10 ℃ after the Beginning of Winter, when noon, temperature was higher with solution 2 pumps that store to the salt pan, freezingly separate out thick Repone K through night, extract the liquid above the thick Repone K the next morning when temperature is low, and whole winter is circulating frozen, separation so repeatedly;
(5) dissolve thick Repone K: the thick Repone K that step (4) obtains is dissolved as saturated solution, clarification with fresh water;
(6) crystalline potassium chloride: ted the solution that step (5) obtains, separate out crystal Repone K, when shining, separate obtaining mother liquor 2 and crystal Repone K to 27～27.5Be;
(7) storage again of mother liquor: the solution 2 that mother liquor 2 that step (6) is obtained and step (2) obtain merges or stores separately, waits use 1 year winter again;
(8) washing, drying: the crystal Repone K that step (6) is obtained removes mother liquor, washing, and drying obtains the Repone K product.
The mother liquor that washing obtains in the step (8) can and the solution that obtains of step (5) merge or ted separately, separate out crystal Repone K.
When the mother liquor 2 that step (6) is obtained stored separately, tedded and directly obtain crystal Repone K 1 year winter.
Make with PVC (polyvinyl chloride) plastic-coated fabric in the employed pond of crystalline potassium chloride in the step (6), method of construction is: launch by the pond design area with PVC (polyvinyl chloride) plastic-coated fabric heat seal or with the PVC plastic-coated fabric, between every limit and the limit overlapped 2 centimetres, be that the alpha-cyanoacrylate fat caking agent of TYPE-W3 is coated with full lap seam with model again, after treating the alpha-cyanoacrylate fat caking agent curing of TYPE-W3, seal fully with the lap seam of igelite caking agent again the bonding mistake of alpha-cyanoacrylate fat caking agent of TYPE-W3.Behind the design area of bonding intact pond, simultaneously be folded into the designed dykes and dams height dimension in pond and add 0.2 meter in addition all around to the center, pond, then outside around build dykes and dams by pond height heap, at last with unnecessary 0.2 meter dig be placed on dykes and dams above, compress with weight, prevent wind.
The method of construction of storage solutions 2 employed grooves is in the step (3): push away 3 meters to 4 meters dark long ditches with dozer according to design capacity, on the level land, do bed course with polyethylene or polypropylene colour bar cloth or blue grey cloth seam shop fixtures according to the total area of bottom of trench limes marginis, seal pre-antiseep between the seam with glue.The total area expansion of on bed course, using PVC (polyvinyl chloride) plastic-coated fabric heat seal again or the PVC plastic-coated fabric being pressed the bottom of trench limes marginis, between every limit and the limit overlapped 2 centimetres, be that the alpha-cyanoacrylate fat caking agent of TYPE-W3 is coated with full lap seam with model again, after treating the alpha-cyanoacrylate fat caking agent curing of TYPE-W3, seal fully with the lap seam of igelite caking agent again the bonding mistake of alpha-cyanoacrylate fat caking agent of TYPE-W3.Behind the bonding intact trench design area, all around with glue with two-layer bonding, by many people bed course and cloth are put into ditch gently according to the length of ditch, compress with weight around the limes marginis.Adopt plastics green house of vegetables mode to build above the ditch, sealing all around prevents the evaporation of storage solutions in the ditch.
The present invention is ingenious utilize great Northwest summer, winter up to the temperature difference of 60 degree and summer up to the steam output of 3460mm, adopt freezing and crystallizing and evaporative crystallization two-step approach to produce the method for crystalline potassium chloride.And what adopt is salt pan big area operation, concentrate so the low yield of the cost utmost point is big, and grade is even.Do not waste resource, rate of recovery height, free from environmental pollution, and be raw material with carnallite floatation method Central Plains depleted tail salt solution, get around heavy long carnallitite and cultivate again and workshop production link again.Method of the present invention adopts is naturally frozen, ted naturally, and purification does not make with medicament one by one, does not need fire coal, substantially need not machinery and power equipment except that taking out halogen, so save energy, there is not environmental pollution, be the environmental protection production method.
Description of drawings
Fig. 1 is the schema of the recovery method of Repone K in the expression carnallite floatation method waste tail liquid of the present invention.
Embodiment
Adopt the mode of specific embodiment further to explain the present invention below, but the present invention is not limited to these embodiment.
Embodiment 1
The concentration that takes by weighing 1260kg is that the tail salt solution of 27Be shines in advance, when shining to 29Be, separate the solution 1 that sodium-chlor obtains 1008kg, obtain the solution 2 of 736kg when tedding solution 1 to 31.3Be, obtain the thick Repone K 86.3kg that KCE content is 47wt% through solution 2 freezing below-10 ℃ again, should be dissolved in the water by thick Repone K again, ted, evaporation, crystallization obtains the crystalline potassium chloride 18.8kg of 90wt%.
Claims (4)
1. the recovery method of Repone K in the carnallite floatation method waste tail liquid is characterized in that it may further comprise the steps:
(1) tail salt solution shines in advance: tail salt solution is shone in advance, and precipitated sodium chloride when shining when concentration is 29Be, separates obtaining sodium-chlor and solution 1;
(2) ted solution 1: solution 1 is continued to ted, separate out low-grade carnallitite, shine to mother liquid concentration and reach 31.2～31.5Be, separate obtaining solution 2;
(3) store: solution 2 is avoided evaporatively being stored in the groove;
(4) freezing, separation: when temperature is reduced to below-10 ℃ after the Beginning of Winter, when noon, temperature was higher with solution 2 pumps that store to the salt pan, freezingly separate out thick Repone K through night, extract the liquid above the thick Repone K the next morning when temperature is low, and whole winter is circulating frozen, separation so repeatedly;
(5) dissolve thick Repone K: the thick Repone K that step (4) obtains is dissolved as saturated solution, clarification with fresh water;
(6) crystalline potassium chloride: ted the solution that step (5) obtains, separate out crystal Repone K, when shining, separate obtaining mother liquor 2 and crystal Repone K to 27～27.5Be;
(7) storage again of mother liquor: the solution 2 that mother liquor 2 that step (6) is obtained and step (2) obtain merges or stores separately, waits use 1 year winter again;
(8) washing, drying: the crystal Repone K that step (6) is obtained removes mother liquor, washing, and drying obtains the Repone K product.
2. method according to claim 1 is characterized in that, the solution that mother liquor that washing obtains in the step (8) and step (5) obtain merges or teds separately, separates out crystal Repone K.
3. method according to claim 1, it is characterized in that, make with PVC (polyvinyl chloride) plastic-coated fabric in the employed pond of crystalline potassium chloride in the step (6), method of construction is: launch by the pond design area with PVC (polyvinyl chloride) plastic-coated fabric heat seal or with the PVC plastic-coated fabric, between every limit and the limit overlapped 2 centimetres, be that the alpha-cyanoacrylate fat caking agent of TYPE-W3 is coated with full lap seam with model again, after treating the alpha-cyanoacrylate fat caking agent curing of TYPE-W3, seal fully with the lap seam of igelite caking agent again the bonding mistake of alpha-cyanoacrylate fat caking agent of TYPE-W3.Behind the design area of bonding intact pond, simultaneously be folded into the designed dykes and dams height dimension in pond and add 0.2 meter in addition all around to the center, pond, then outside around build dykes and dams by pond height heap, at last with unnecessary 0.2 meter dig be placed on dykes and dams above, compress with weight, prevent wind.
4. method according to claim 1, it is characterized in that, the method of construction of storage solutions 2 employed grooves is in the step (3): push away 3 meters to 4 meters dark long ditches with dozer according to design capacity, on the level land, do bed course with polyethylene or polypropylene colour bar cloth or blue grey cloth seam shop fixtures according to the total area of bottom of trench limes marginis, seal pre-antiseep between the seam with glue.The total area expansion of on bed course, using PVC (polyvinyl chloride) plastic-coated fabric heat seal again or the PVC plastic-coated fabric being pressed the bottom of trench limes marginis, between every limit and the limit overlapped 2 centimetres, be that the alpha-cyanoacrylate fat caking agent of TYPE-W3 is coated with full lap seam with model again, after treating the alpha-cyanoacrylate fat caking agent curing of TYPE-W3, seal fully with the lap seam of igelite caking agent again the bonding mistake of alpha-cyanoacrylate fat caking agent of TYPE-W3.Behind the bonding intact trench design area, all around with glue with two-layer bonding, by many people bed course and cloth are put into ditch gently according to the length of ditch, compress with weight around the limes marginis.Adopt plastics green house of vegetables mode to build above the ditch, sealing all around prevents the evaporation of storage solutions in the ditch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410073691 CN1274597C (en) | 2004-09-01 | 2004-09-01 | Recovery method for potassium chloride from waste tail liquid by carnallite flotation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410073691 CN1274597C (en) | 2004-09-01 | 2004-09-01 | Recovery method for potassium chloride from waste tail liquid by carnallite flotation process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1587047A true CN1587047A (en) | 2005-03-02 |
| CN1274597C CN1274597C (en) | 2006-09-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410073691 Expired - Fee Related CN1274597C (en) | 2004-09-01 | 2004-09-01 | Recovery method for potassium chloride from waste tail liquid by carnallite flotation process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1274597C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2305067C1 (en) * | 2005-12-02 | 2007-08-27 | Открытое Акционерное Общество "Корпорация Всмпо-Ависма" | Method of preparation of the carnallite for electrolysis |
| CN102205976A (en) * | 2011-04-08 | 2011-10-05 | 何茂雄 | Recovery method of potassium ions in flotation tailing liquid and tailing |
| CN102491372A (en) * | 2011-11-30 | 2012-06-13 | 化工部长沙设计研究院 | Method of producing potassium chloride from reverse flotation tailings of carnallite |
| CN102583446A (en) * | 2012-02-13 | 2012-07-18 | 河北工业大学 | Method for preparing potassium chloride through decomposing carnallite by concentrated brine |
| CN102923735A (en) * | 2012-09-28 | 2013-02-13 | 新疆昆金矿业有限责任公司 | Method for preparing potassium chloride through highland salt lake raw brine salt pan process |
| CN109516477A (en) * | 2018-12-26 | 2019-03-26 | 青海盐湖工业股份有限公司 | A kind of method and system using tail salt production potassium chloride |
| CN110590412A (en) * | 2019-10-17 | 2019-12-20 | 青海盐湖工业股份有限公司 | Method for recovering water bath dedusting wastewater in potash fertilizer production |
| CN115788513A (en) * | 2023-01-17 | 2023-03-14 | 煤炭工业太原设计研究院集团有限公司 | Supporting waterproof structure and method for inclined shaft at junction of mudstone and carnallite deposits |
-
2004
- 2004-09-01 CN CN 200410073691 patent/CN1274597C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2305067C1 (en) * | 2005-12-02 | 2007-08-27 | Открытое Акционерное Общество "Корпорация Всмпо-Ависма" | Method of preparation of the carnallite for electrolysis |
| CN102205976A (en) * | 2011-04-08 | 2011-10-05 | 何茂雄 | Recovery method of potassium ions in flotation tailing liquid and tailing |
| CN102491372A (en) * | 2011-11-30 | 2012-06-13 | 化工部长沙设计研究院 | Method of producing potassium chloride from reverse flotation tailings of carnallite |
| CN102583446A (en) * | 2012-02-13 | 2012-07-18 | 河北工业大学 | Method for preparing potassium chloride through decomposing carnallite by concentrated brine |
| CN102583446B (en) * | 2012-02-13 | 2013-07-24 | 河北工业大学 | Method for preparing potassium chloride through decomposing carnallite by concentrated brine |
| CN102923735A (en) * | 2012-09-28 | 2013-02-13 | 新疆昆金矿业有限责任公司 | Method for preparing potassium chloride through highland salt lake raw brine salt pan process |
| CN109516477A (en) * | 2018-12-26 | 2019-03-26 | 青海盐湖工业股份有限公司 | A kind of method and system using tail salt production potassium chloride |
| CN110590412A (en) * | 2019-10-17 | 2019-12-20 | 青海盐湖工业股份有限公司 | Method for recovering water bath dedusting wastewater in potash fertilizer production |
| CN115788513A (en) * | 2023-01-17 | 2023-03-14 | 煤炭工业太原设计研究院集团有限公司 | Supporting waterproof structure and method for inclined shaft at junction of mudstone and carnallite deposits |
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| Publication number | Publication date |
|---|---|
| CN1274597C (en) | 2006-09-13 |
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