CN1052705C - Process for producing potassium chloride from carnallite - Google Patents
Process for producing potassium chloride from carnallite Download PDFInfo
- Publication number
- CN1052705C CN1052705C CN97103513A CN97103513A CN1052705C CN 1052705 C CN1052705 C CN 1052705C CN 97103513 A CN97103513 A CN 97103513A CN 97103513 A CN97103513 A CN 97103513A CN 1052705 C CN1052705 C CN 1052705C
- Authority
- CN
- China
- Prior art keywords
- carnallitite
- sodium
- chlor
- carnallite
- add
- 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.)
- Expired - Lifetime
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 12
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 12
- 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 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 20
- 238000005188 flotation Methods 0.000 claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 19
- 241001131796 Botaurus stellaris Species 0.000 claims description 10
- 238000005695 dehalogenation reaction Methods 0.000 claims description 9
- 150000002193 fatty amides Chemical group 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- -1 alkyl morpholine Chemical compound 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Natural products C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims 2
- 238000005516 engineering process Methods 0.000 abstract description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000011780 sodium chloride Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 230000008719 thickening Effects 0.000 abstract 2
- 229910052736 halogen Inorganic materials 0.000 abstract 1
- 150000002367 halogens Chemical class 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 26
- 239000002245 particle Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000008396 flotation agent Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 241000272875 Ardeidae Species 0.000 description 1
- LBPACUJFGRCWDF-UHFFFAOYSA-L Cl[Mg]Cl.[Na] Chemical compound Cl[Mg]Cl.[Na] LBPACUJFGRCWDF-UHFFFAOYSA-L 0.000 description 1
- 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 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention belongs to the technical field of a technology which takes carnallite ores or products as raw materials to produce potassium chloride products. The technology is characterized in that the technological flow comprises the following working procedures: pulp regulation, reverse flotation, thickening 1, halogen removal, decomposition crystallization, thickening 2, filtration, drying and potassium chloride product acquisition; the ratio of solids to liquid is from 15 to 40% in the pulp regulating working procedure; floatation agents in the working procedure of reverse flotation are sodium chloride collecting agents; and in the working procedure of decomposition crystallization, the quantity of added water is from 700 to 1100 kilograms per ton of carnallite raw materials, and the quantity of added magnesium chloride unsaturated solution is from 1100 to 6000 kilograms per ton of carnallite fine materials. The method has the advantages of coarse granularity of products, easy drying, stable and reliable product quality, low energy consumption, low production cost, simple technology, etc. Moreover, the product quality is free from the limitations of the grade and the quality of raw materials, and equipment can not be corroded by water.
Description
The invention belongs to carnallite or product is raw material production Repone K product Technology field.
Existing is that the method for raw material production Repone K mainly contains thermosoling with the carnallitite.Flotation process, three kinds of processing methodes of cold decomposition and crystallization method.The advantage of thermosoling is a Repone K yield height, and constant product quality is not subjected to the influence of ore quality, and its shortcoming is the energy consumption height, and equipment corrosion is serious, the product cost height.Flotation process is to get artificial sylvite after carnallitite is decomposed de-magging, makes the technology of collecting agent flotation Repone K again with stearylamine, and this method technology is simple, but shortcoming is to obtain the chlorization product fine size, product drying dehydration difficulty.Cold decomposition and crystallization method is the new technology that development in recent years is got up, it is after carnallitite is added water decomposition crystallization de-magging, add water washing and directly obtain the Repone K crystalline product, its advantage is that energy consumption is low, good product quality, cost is low, and its shortcoming is to carnallitite grade requirement height, it is responsive that Repone K product yield and quality are influenced by the carnallitite head grade, and low-grade carnallite is needed could use after enrichment is handled.
The objective of the invention is the shortcoming at above-mentioned three kinds of technologies existence, absorb the advantage of technologies such as flotation process and cold decomposition and crystallization method, design studies goes out a kind of new processing method---reverse flotation decomposition and crystallization method.It is thick that this method has a product granularity, and easily dry, quality product is not limited by ore quality, and advantage such as steady quality is reliable, and energy consumption is low, and production cost is low, and equipment corrosion is little, and technology is simple.
The technical scheme of this invention is: technical process is for sizing mixing → reverse flotation → dense (one) → dehalogenation → decomposition and crystallization → dense (two) → filtration → washing dehydration → drying → Repone K product.The solid-to-liquid ratio of the operation of sizing mixing is 15-40% (weight ratio), the flotation agent of reverse flotation operation is the sodium-chlor collecting agent, decomposition and crystallization operation amount of water is 700-1100 kilogram/ton carnallitite fine fodder, and adding the magnesium chloride unsaturated solution is 1100-6000 kilogram/ton carnallitite fine fodder.The operation of sizing mixing is the process that the saturated bittern that carnallite adds a certain amount of Repone K or carnallitite is made it to reach certain solid-to-liquid ratio, the carnallitite raw material: the bittern amount is called solid-to-liquid ratio (weight ratio) and is 15-40%.The reverse flotation operation is gained the name at the flotation operation, and the reverse flotation operation is to floatingly select sodium chloride as impurity.Stay the process of carnallitite fine fodder, sodium-chlor collecting agent such as alkyl morpholine, fatty amide.Preferably selecting its add-on of fatty amide for use is 100-400 gram/ton carnallitite raw material, and alkyl morpholine is a 15-150 gram/ton carnallitite raw material, and alkyl morpholine mixes with fatty amide to use and is 15-400 gram/ton carnallitite raw material.Often in the operation of sizing mixing, add the sodium-chlor collecting agent convenient in the production.Dense (one) operation is that the carnallitite slurry after removing sodium chloride as impurity is carried out the spissated process of sedimentation, is beneficial to the centrifugal dehalogenation of dehalogenation operation.The decomposition and crystallization operation is that the carnallitite fine fodder behind the dehalogenation is added the process that water or magnesium chloride unsaturated solution decompose recrystallize, its amount of water is 700-1100 kilogram/ton carnallitite fine fodder, adding the magnesium chloride unsaturated solution is 1100-6000 kilogram/ton carnallitite fine fodder, be the water or the 1100-6000 kilogram magnesium chloride unsaturated solution of 1 ton of about 700-1100 kilogram of carnallitite fine fodder adding behind the dehalogenation, also water or magnesium chloride unsaturated solution can be mixed adding.Decomposition is that carnallitite is decomposed, and crystallization is the crystalline potassium chloride crystal, enters dense (two) operation after the decomposition and crystallization again.Dense (two) operation is that the Repone K slurry is further concentrated the process of removing bittern, and filtering operation is the process of further sloughing mother liquor.Can add the washing dehydration operation again after filtering operation, this operation is to add washing decon such as sodium-chlor, magnesium chloride etc., slough residual moisture content, the process of further improving the quality of products, this operation such as quality product have reached the user quality requirement, and then this operation can be omitted, and the Repone K work in-process that have certain moisture content after the filtration can directly enter drying process, remove residual moisture content, can obtain exsiccant Repone K product.
In the production, add a certain amount of flotation agent when the carnallitite raw material being sized mixing and carry out reverse flotation, because flotation agent contains the fatty amide of 8-12 carbochain sodium-chlor is had collecting effect preferably, so it can effectively remove the sodium chloride as impurity in the carnallitite raw material with bittern.In the reverse flotation operation successively through roughly selecting, selected, just can remove a large amount of sodium chloride as impurity, must the carnallitite fine fodder.In the reverse flotation operation, in the carnallitite slurry, add the sodium-chlor collecting agent, introducing air in the slurry again, then the water layer on sodium-chlor surface breaks rapidly, and and bubble be closely linked and rise to the ore pulp surface, the foam of these band sodium-chlor ore particles is scraped, just only contain the low-sodium carnalite ore deposit in the remaining ore pulp.Remove part bittern through dense (one), again dehalogenation slough bittern get final product the carnallitite concentrate of low sodium.Decomposition and crystallization is to utilize cold decomposition and crystallization principle to produce the method for coarse particles Repone K, in this operation,, promptly control the crystallization condition of Repone K if can control the carnallitite dissolution rate well, make the dissolution rate of carnallitite too not fast, just can obtain thicker potassium chloride particle.Obtaining bigger particulate potassium chloride is to guarantee that the back can be dry smoothly, remove the condition of moisture content fully, potassium chloride particle owing to generation in the existing technology is too thin, can not be dry smoothly, product water content height, thereby influence quality product and benefit, technology of the present invention has solved this difficult problem effectively.Filter the back quality product and just can reach after drying, no longer add the washing dehydration operation after then filtering, otherwise, require height as quality product, can not reach the quality product requirement after drying, increase the washing dehydration operation again after then filtering, the bittern of discharging can be recycled, and the sodium-chlor slurry can use it for anything else.
The present invention at first makes with extra care raw material, solved the defective that quality product is restricted by head grade, found outlet for the utilization of low grade material, this technology has increased the crystalline particle of product in addition, solve this difficult problem of drying and dehydrating difficulty effectively, improved quality product.This technology is all carried out except that drying at normal temperatures and pressures, and is easy to operate, and equipment corrosion is little, and hear rate is low, and product cost is low, and good economic and social benefit is arranged.
Accompanying drawing 1 is a process flow diagram of the present invention.
Embodiment one: get 250 kilograms of carnallitite raw materials, it is 21.7% that raw material is formed KCE content, and magnesium chloride is 27.74%, and sodium-chlor is 17.95%, sizes mixing with 1000 kilograms of carnallitite saturated bitterns.The sodium-chlor collecting agent that the reverse flotation operation adds 25 gram fatty amides behind twice of reverse flotation, carries out dense (one) operation through sedimentation, gets the carnallitite fine fodder behind the dehalogenation.The carnallitite fine fodder is 215 kilograms, and it forms Repone K is 25.20%, and magnesium chloride is 32.19%, and sodium-chlor is 5.88%.With 160 kg of water decomposition and crystallization, through dense (two), filter the Repone K work in-process, it forms Repone K is 92.65%, sodium-chlor 5.91%, insolubles impurity are 1.44%.Water gets 40 kilograms of Repone K products to the washing of Repone K work in-process, dehydration, drying again, and it consists of Repone K 98.42%, insolubles 1.58%.
Embodiment two: get 100 kilograms of carnallitite raw materials, size mixing with 350 kilograms of bittern.The reverse flotation operation adds 20 grams and contains the fatty amide of 8-12 carbochain and the sodium-chlor collecting agent of 3 gram alkyl morpholines, gets 87 kilograms of carnallitite fine fodders again behind dense (one), dehalogenation.With 160 kilograms of magnesium chloride unsaturated solutions the carnallitite fine fodder is carried out decomposition and crystallization, again through dense (two), filtration, drying just can get 17 kilograms of Repone K products.
Claims (3)
1. process for producing potassium chloride from carnallite is characterized in that:
(1) technical process: (one) → dehalogenation → decomposition and crystallization of sizing mixing → reverse flotation → dense → dense (two) → filtration → drying → Repone K product;
(2) operation of sizing mixing is that the carnallitite raw material is added in Repone K saturated bittern or the carnallitite saturated bittern, and the solid-to-liquid ratio of the slurries that are mixed with is 15～40% (weight ratios); The reverse flotation operation is to add the sodium-chlor collecting agent in above-mentioned slurries, floatingly selects solid impurities such as sodium-chlor, stays the carnallitite fine fodder; The decomposition and crystallization operation is to add water in above-mentioned carnallitite fine fodder, and amount of water is 700～1100 kilograms of/ton carnallitite fine fodders, adds the magnesium chloride unsaturated solution, and add-on is 1100～6000 kilograms of/ton carnallitite fine fodders.
2. process for producing potassium chloride from carnallite according to claim 1 is characterized in that increasing the washing dehydration operation after filtering operation.
3. process for producing potassium chloride from carnallite according to claim 1 and 2 is characterized in that above-mentioned sodium-chlor collecting agent is fatty amide, alkyl morpholine or the mixture of the two; When the sodium-chlor collecting agent is fatty amide, its add-on is 100～400 gram/ton carnallitite raw materials, when the sodium-chlor collecting agent is alkyl morpholine, its add-on is 15～150 gram/ton carnallitite raw materials, when the sodium-chlor collecting agent was the mixture of alkyl morpholine and fatty amide, its add-on was 15～400 gram/ton carnallitite raw materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103513A CN1052705C (en) | 1997-03-13 | 1997-03-13 | Process for producing potassium chloride from carnallite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103513A CN1052705C (en) | 1997-03-13 | 1997-03-13 | Process for producing potassium chloride from carnallite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1180046A CN1180046A (en) | 1998-04-29 |
| CN1052705C true CN1052705C (en) | 2000-05-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97103513A Expired - Lifetime CN1052705C (en) | 1997-03-13 | 1997-03-13 | Process for producing potassium chloride from carnallite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1052705C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384737C (en) * | 2004-06-09 | 2008-04-30 | 华东理工大学 | Potassium chloride production method with low calcium sulfate content |
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| CN1120803C (en) * | 1999-11-19 | 2003-09-10 | 乔希海 | Process for producing potassium chloride from alkaline slag and potassium feldspar |
| EP1699738B1 (en) * | 2003-12-31 | 2010-12-01 | Council of Scientific and Industrial Research | SIMULTANEOUS RECOVERY OF POTASSIUM CHLORIDE AND KCl ENRICHED EDIBLE SALT |
| CN100364891C (en) * | 2004-12-22 | 2008-01-30 | 江进兴 | Method for preparing potassium chloride by sunshine thermo solvation |
| CN101157460B (en) * | 2007-08-28 | 2010-09-01 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride by employing sulfate type salt lake potassium-containing brine |
| CN101474598B (en) * | 2009-01-23 | 2012-10-24 | 云南省化工研究院 | Method for flotation of potassium chloride from potassium salt mine |
| CN101723409B (en) * | 2009-12-18 | 2011-09-07 | 中蓝连海设计研究院 | Method for preparing potassium chloride with inferior carnallite |
| CN103193252B (en) * | 2013-04-24 | 2014-06-25 | 化工部长沙设计研究院 | Method for producing potassium chloride by adopting carnallite hot-melt brine |
| CN104058427B (en) * | 2014-07-03 | 2016-05-18 | 青海盐湖工业股份有限公司 | A kind of high-grade KCl production system and method thereof |
| CN107162017B (en) * | 2017-07-05 | 2019-03-15 | 青海盐湖工业股份有限公司 | The recovery and processing system and method for mother liquor in a kind of production of potash fertilizer |
| CN107555451B (en) * | 2017-08-28 | 2020-06-12 | 青海盐湖工业股份有限公司 | Method for producing potassium chloride by using tail salt ore |
| CN107572552B (en) * | 2017-10-11 | 2020-03-24 | 青海盐湖工业股份有限公司 | Production process for preparing potassium chloride from carnallite |
| CN109541127A (en) * | 2018-12-19 | 2019-03-29 | 青海盐湖工业股份有限公司 | The method that a kind of pair of saturated potassium chloride solution carries out assay |
| CN109626398A (en) * | 2019-02-13 | 2019-04-16 | 青海盐湖工业股份有限公司 | A kind of method of essence potassium slurry concentration dehalogenation |
| CN111661855B (en) * | 2019-03-06 | 2021-07-23 | 青海盐湖工业股份有限公司 | Method and system for producing potassium chloride by recycling byproducts |
| CN112299450B (en) * | 2020-11-18 | 2023-02-28 | 青海盐湖工业股份有限公司 | Method for preparing potassium chloride by grading crude potassium and potassium chloride prepared by applying method |
| CN117105244A (en) * | 2023-09-05 | 2023-11-24 | 青海盐湖工业股份有限公司 | Method for preparing potassium chloride by double flotation and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057208A (en) * | 1984-09-25 | 1991-10-15 | Kali Und Salz Aktiengesellschaft | Method for the production of potassium chloride with K2 O content of more than 55 weight percent |
-
1997
- 1997-03-13 CN CN97103513A patent/CN1052705C/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057208A (en) * | 1984-09-25 | 1991-10-15 | Kali Und Salz Aktiengesellschaft | Method for the production of potassium chloride with K2 O content of more than 55 weight percent |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384737C (en) * | 2004-06-09 | 2008-04-30 | 华东理工大学 | Potassium chloride production method with low calcium sulfate content |
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| Publication number | Publication date |
|---|---|
| CN1180046A (en) | 1998-04-29 |
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Owner name: QINGHAI SALT LAKE INDUSTRIAL CO., LTD. Free format text: FORMER NAME: YANHU INDUSTRY GROUP CO., LTD. QINGHAI |
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Address after: 816000 No. 28, the Yellow River Road, Golmud, Qinghai Patentee after: Qinghai Salt Lake Industry Co., Ltd. Address before: The Yellow River City, Qinghai province 816000 Erythrophleum Road No. 1 Patentee before: Yanhu Industry Group Co., Ltd. Qinghai |
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Granted publication date: 20000524 |