CN100384737C - Preparing method for potassium chloride with low calcium sulfate content - Google Patents
Preparing method for potassium chloride with low calcium sulfate content Download PDFInfo
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- CN100384737C CN100384737C CNB200410025015XA CN200410025015A CN100384737C CN 100384737 C CN100384737 C CN 100384737C CN B200410025015X A CNB200410025015X A CN B200410025015XA CN 200410025015 A CN200410025015 A CN 200410025015A CN 100384737 C CN100384737 C CN 100384737C
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- flotation
- potassium chloride
- repone
- preparation
- calcium sulfate
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Abstract
The present invention relates to a preparation method for potassium chloride of the industrial grade. On the basis of the deep research of the distribution and the existing state of all groups of carnallite ores, the inventor proposes a method of grading, cold decomposition, direct flotation or grading, reverse flotation and cold crystallization to prepare industrial potassium chloride. The preparation method for potassium chloride of the present invention has the advantages that the preparation method for potassium chloride is simple and easily feasible, is suitable for large-scale industrialized production, etc.; meanwhile, the content of calcium sulfate in potassium chloride products prepared by the preparation method of the present invention is not more than 0.2%, so the potassium chloride products can completely reach the quality of potassium chloride of the industrial grade.
Description
Technical field
The present invention relates to a kind of Repone K production method, specifically, relating to a kind of is raw material with the carnallitite, adopts the method for direct flotation or reverse flotation-cold crystallization prepared Repone K.
Background technology
China's salt lake resources is abundant, and wherein Cha Er sweat salt lake has abundant Repone K resource (it exists with the carnallite form), and reserves reach 1.45 hundred million tons, account for national explored salt lake reserves 97%.
Be in the technology of feedstock production Repone K with the carnallitite, direct flotation or reverse flotation-cold crystallization method is generally to adopt both at home and abroad at present and the most advanced technology.The key step of reverse flotation-cold crystallization method is: floatation equipment is sized mixing afterwards, sent into to carnallite and bittern, adopting alkyl morpholine is that flotation reagent carries out flotation and obtains refined carnallite (or claiming low-sodium carnalite), and low-sodium carnalite obtains the Repone K product after removing magnesium chloride through cold crystallization.Solved at present the sodium-chlor that removes in the carnallitite and the technical problem of magnesium chloride in this technology preferably, yet the direct flotation of (containing 1～2% calcium sulfate in the carnallitite) problem that removes of calcium sulfate in the carnallitite-no matter or reverse flotation-cold crystallization Fa-as yet have not been obtained fine solution.So just cause calcium sulphate content higher (can't reach the requirement of technical grade Repone K) in the present Repone K product, this brings very big difficulty for expansion Repone K Application Areas.Therefore, resolve in the Repone K production process problem that removes of calcium sulfate and become the key that promotes the Repone K quality product.
" chemical industry mineral and processing " the 8th phase in 2000 has been reported employing QHS-2 and AN compound compound drug flotation removing calcium sulfate, and its effect is undesirable, and room for improvement is still arranged, and can not reach technical grade Repone K product quality requirement.
Summary of the invention
The present invention needs technical problem to be: solve the problem that calcium sulfate removes in the Repone K production process.In other words, provide a kind of method for preparing technical grade Repone K.
The contriver finds that by the existence of research calcium sulfate in carnallite 95% above calcium sulfate mainly exists with the particle below the 100 μ m, and wherein granularity accounts for 78.23% below 70 μ m.Research also find calcium sulfate in carnallite with the small-particle Individual existence, only account for 5% or still less and be wrapped in calcium sulfate in sodium-chlor and the refined carnallite particle.Find that according to this contriver has proposed the Repone K production method of classification-flotation, content≤0.5% of calcium sulfate in the Repone K that makes with this method can reach the quality of technical grade Repone K fully.
Technical scheme:
The preparation method of the said Repone K of the present invention, it comprises the steps:
To in the saturated bittern medium, separate and remove particle diameter less than 100 μ m particulate carnallitites, send into flotation machine with the reverse flotation agent after 1: 4 mixing is sized mixing by weight with saturated bittern and carry out flotation, flotation time is 0.5～2 hour, low-sodium carnalite through making behind the reverse flotation is obtained the Repone K product again after cold crystallization, washing and drying, wherein, the add-on of reverse flotation agent is 8 gram/ton saturated bitterns;
Wherein: said reverse flotation agent is as follows:
N-hexadecyl morpholine 85wt%
C
12H
25-NH
2 10wt％
Molecular weight is 400～20000 polyoxyethylene glycol 3wt%
Sodium hexametaphosphate 99 2wt%
Or
N-C
20Alkyl morpholine 85wt%
C
12H
25-NH
2 10wt％
Molecular weight 1000～30000 polyglycol ether 3wt%
Sodium hexametaphosphate 99 2wt%
Used saturated bittern is formed: KCl:0.27%, MgCl
2: CaSO 33.08%,
4: 0.14%.
In the present invention, the preparation of reverse flotation agent is: raw material is mixed according to the above ratio get final product.
The present invention is by to each component cloth in the carnallite and there is the further investigation of situation, classification-cold decomposition-direct floatation or the classification-reverse flotation-cold crystallization method that proposed prepares Repone K, the said Repone K preparation method of the present invention has simple, be suitable for advantages such as heavy industrialization, adopt content≤0.5% of calcium sulfate in the Repone K that preparation method of the present invention makes simultaneously, can reach the quality of technical grade Repone K fully.
Embodiment
The invention will be further described below by embodiment, and the cited case does not influence protection scope of the present invention:
Embodiment 1
Raw material bittern and carnallitite are taken from Cha Erhan salt lake, Qinghai.
Get the thick carnallitite of 1000 grams, sieve with 200 order mesh screens in saturated bittern, obtain sieving about 770 grams of carnallite, sieve is about 205 grams in ore deposit down.
Get above-mentioned upper strata carnallite 500 gram, be added in the 2000 gram saturated bitterns, stir about adds composite chemical for floatating 0.016 gram after 1 minute, mix 15 minutes earlier after, beginning bubbling flotation 20 minutes is scraped then and is steeped after 15 minutes, stops flotation.Filtered, weigh in gained foam layer ore deposit and bittern chats, obtain about 370 grams of lower floor's low-sodium carnalite, calcium sulphate content is 0.38%, and low-sodium carnalite can get the Repone K product after cold crystallization technology, and sulfur acid calcium is 0.45% in the Repone K.
Flotation reagent is formulated as follows:
N-hexadecyl morpholine 85%,
C
12Aliphatic amide (C
12H
25-NH
2) 10%,
Polyoxyethylene glycol (molecular weight: 400～20000) 3%,
Sodium hexametaphosphate 99 2%.
Embodiment 2
Raw material bittern and carnallitite are taken from Cha Erhan salt lake, Qinghai.
Get the thick carnallitite of 1000 grams, sieve with 200 order mesh screens in saturated bittern, obtain sieving about 770 grams of carnallite, sieve is about 205 grams in ore deposit down.
Get above-mentionedly greater than 200 purpose carnallites 500 gram, mix rapidly and separates with 2000 gram fresh water, obtaining mainly with sodium-chlor, Repone K, calcium sulfate is that the solid particulate about 200 of main component restrains; With gained mixture and saturated bittern with 30% ratio mixing, add flotation reagent 500 gram/ton bittern, stir after 0.5 hour flotation and obtain about 60 grams of potassium chloride particle, further wash, filter, obtain the Repone K product after the drying, calcium sulphate content is 0.18% in the Repone K.
Flotation reagent is formulated as follows:
The C of 10wt%
8The hydrochloride (C of aliphatic amide
8H
17-NH
2HCl) solution 85%,
Pine camphor oil (No. 2 oil) 10%,
C
12Acid amides 5%.
Embodiment 3
Raw material bittern and carnallitite are taken from Cha Erhan salt lake, Qinghai.
Get the thick carnallitite of 1000 grams, sieve with 200 order mesh screens in saturated bittern, obtain sieving about 770 grams of carnallite, sieve is about 205 grams in ore deposit down.
Get above-mentioned upper strata carnallite 500 gram, be added in the 2000 gram saturated bitterns, stir about adds composite chemical for floatating 0.016 gram after 1 minute, mix 15 minutes earlier after, beginning bubbling flotation 20 minutes is scraped then and is steeped after 15 minutes, stops flotation.Filtered, weigh in gained foam layer ore deposit and bittern chats, obtain about 370 grams of lower floor's low-sodium carnalite, calcium sulphate content is 0.38%, and low-sodium carnalite can get the Repone K product after cold crystallization technology, and sulfur acid calcium is 0.45% in the Repone K.
Flotation reagent is formulated as follows:
N-C
20Alkyl morpholine 85%,
C
12Aliphatic amide (C
12H
25-NH
2) 10%,
Polyglycol ether (molecular weight: 1000～30000) 3%,
Sodium hexametaphosphate 99 2%.
Embodiment 4
Raw material bittern and carnallitite are taken from Cha Erhan salt lake, Qinghai.
Get the thick carnallitite of 1000 grams, sieve with 200 order mesh screens in saturated bittern, obtain sieving about 770 grams of carnallite, sieve is about 205 grams in ore deposit down.
Get above-mentioned carnallite 500 grams, mix rapidly and separate with 2000 gram fresh water, obtaining mainly is about 200 grams of solid particulate of main component with sodium-chlor, Repone K, calcium sulfate; With gained mixture and saturated bittern with 30% ratio mixing, add flotation reagent 500 gram/ton bittern, stir after 0.5 hour flotation and obtain about 60 grams of potassium chloride particle, further wash, filter, obtain the Repone K product after the drying, calcium sulphate content is 0.18 in the Repone K.
Flotation reagent is formulated as follows:
10wt%C
20The hydrochloride (C of aliphatic amide
20H
17-NH
2HCl) solution 85%,
Pine camphor oil (No. 2 oil) 10%,
C
12Acid amides 5%.
Claims (1)
1. a Repone K preparation method is characterized in that, it comprises the steps: said preparation method
To in the saturated bittern medium, separate and remove particle diameter less than 100 μ m particulate carnallitites, send into flotation machine with the reverse flotation agent after 1: 4 mixing is sized mixing by weight with saturated bittern and carry out flotation, flotation time is 0.5～2 hour, low-sodium carnalite through making behind the reverse flotation is obtained the Repone K product again after cold crystallization, washing and drying, wherein, the add-on of reverse flotation agent is 8 gram/ton saturated bitterns;
Wherein: said reverse flotation agent is as follows:
N-hexadecyl morpholine 85wt%
C
12H
25-NH
2 10wt％
Molecular weight is 400～20000 polyoxyethylene glycol 3wt%
Sodium hexametaphosphate 99 2wt%
Or
N-C
20Alkyl morpholine 85wt%
C
12H
25-NH
2 10wt％
Molecular weight 1000～30000 polyglycol ether 3wt%
Sodium hexametaphosphate 99 2wt%
Used saturated bittern is formed: KCl:0.27%, MgCl
2: CaSO 33.08%,
4: 0.14%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410025015XA CN100384737C (en) | 2004-06-09 | 2004-06-09 | Preparing method for potassium chloride with low calcium sulfate content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410025015XA CN100384737C (en) | 2004-06-09 | 2004-06-09 | Preparing method for potassium chloride with low calcium sulfate content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1583565A CN1583565A (en) | 2005-02-23 |
| CN100384737C true CN100384737C (en) | 2008-04-30 |
Family
ID=34601101
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410025015XA Expired - Fee Related CN100384737C (en) | 2004-06-09 | 2004-06-09 | Preparing method for potassium chloride with low calcium sulfate content |
Country Status (1)
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|---|---|
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100411988C (en) * | 2005-09-23 | 2008-08-20 | 清华大学 | Calcium removing and purification method of industrial potassium chloride |
| CN1927715B (en) * | 2006-06-16 | 2012-05-23 | 魏学民 | Method of removing calcium sulphate from carnallite |
| 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 |
| CN101811095B (en) * | 2010-04-23 | 2013-06-19 | 攀钢集团钢铁钒钛股份有限公司 | Floatation desulphurization method of acid-leaching vanadium-extracted residues |
| CN102417192B (en) * | 2011-08-26 | 2014-04-16 | 封昊 | Process for processing potassium chloride raw material for making ion membrane potassium hydroxide |
| CN102815725A (en) * | 2012-07-18 | 2012-12-12 | 中蓝连海设计研究院 | Process for preparing potassium chloride by using carnallite containing calcium sulfate |
| FR2999455B1 (en) * | 2012-12-19 | 2016-07-15 | Solvay | METHOD FOR SEPARATING CALCIUM CARBONATE AND GYPSUM |
| CN104492609A (en) * | 2014-11-04 | 2015-04-08 | 中蓝连海设计研究院 | Calcium sulfate collecting agent and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4504092A (en) * | 1981-03-05 | 1985-03-12 | Mines De Potasse D'alsace S.A. | Treatment of carnallitic ores |
| CN1052705C (en) * | 1997-03-13 | 2000-05-24 | 青海盐湖工业集团有限公司 | Process for producing potassium chloride from carnallite |
-
2004
- 2004-06-09 CN CNB200410025015XA patent/CN100384737C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4504092A (en) * | 1981-03-05 | 1985-03-12 | Mines De Potasse D'alsace S.A. | Treatment of carnallitic ores |
| CN1052705C (en) * | 1997-03-13 | 2000-05-24 | 青海盐湖工业集团有限公司 | Process for producing potassium chloride from carnallite |
Non-Patent Citations (4)
| Title |
|---|
| 反浮选一冷结晶生产氮化钾工艺控制的探讨. 汪贵元.海湖盐与化工，第31卷第3期. 2002 |
| 反浮选一冷结晶生产氮化钾工艺控制的探讨. 汪贵元.海湖盐与化工，第31卷第3期. 2002 * |
| 浮选法生产氯化钾工艺在生产实践中的应用. 李承宝.海湖盐与化工，第28卷第2期. 1999 |
| 浮选法生产氯化钾工艺在生产实践中的应用. 李承宝.海湖盐与化工，第28卷第2期. 1999 * |
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| Publication number | Publication date |
|---|---|
| CN1583565A (en) | 2005-02-23 |
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Owner name: EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY; Q Free format text: FORMER NAME OR ADDRESS: EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY; QINGHAI YANHU INDUSTRY GROUP CO., LTD. |
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Address after: No. 130, Meilong Road, Shanghai, Xuhui District: 200237 Co-patentee after: Qinghai Yanhu Industry Group Co., Ltd. Patentee after: East China University of Science and Technology Address before: No. 130, Meilong Road, Shanghai, Xuhui District: 200237 Co-patentee before: Yanhu Industry Group Co., Ltd. Qinghai Patentee before: East China University of Science and Technology |
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Correction item: Patentee Correct: Yanhu Industry Group Co., Ltd. Qinghai False: Qinghai Yanhu Industry Group Co., Ltd. Number: 46 Page: 1501 Volume: 24 |
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Free format text: CORRECT: PATENTEE; FROM: QINGHAI SALT LAKE INDUSTRY GROUP CO.LTD. TO: QINGHAI YANHU INDUSTRY GROUP CO., LTD. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080430 Termination date: 20150609 |
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