CN1038833C - Method for prepn. of potassium sulphate - Google Patents
Method for prepn. of potassium sulphate Download PDFInfo
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- CN1038833C CN1038833C CN93100790A CN93100790A CN1038833C CN 1038833 C CN1038833 C CN 1038833C CN 93100790 A CN93100790 A CN 93100790A CN 93100790 A CN93100790 A CN 93100790A CN 1038833 C CN1038833 C CN 1038833C
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- potassium
- mother liquor
- sulfate
- soft
- schoenite
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Abstract
The present invention relates to a method for preparing potassium sulfate. Raw mineral material containing potassium, magnesium, sulfate radical, sodium and chlorine ions is mixed with soft potassium mother liquor and potassium sulfate mother liquor, and the certain weight ratio of potassium to magnesium to sulfate radical to water in the mixture is controlled; the mixture carries out the thermosol reaction and the liquid and solid separation by heat preservation, and then crude halite and saturated solution are prepared. The saturated solution is crystallized by cooling to prepare soft potassium mixed salt containing schoenite and chloratum kalium, and carries out solid and liquid separation to prepare mixed salt and soft potassium mother liquor; the soft potassium mother liquor can return back to the thermosol stage; the water is added to the soft potassium to react, and then the potassium sulfate can be prepared. The present invention can be used for preparing potassium sulfate with high quality, the utilization rate of the potassium and the sulfate radical is high, and the technological process is short and reasonable.
Description
The present invention relates to a kind of method of utilizing mineral wealth to produce vitriolate of tartar.
With mineral be raw material produce vitriolate of tartar preferably technological process be to make high-quality schoenite earlier, then with high-grade Repone K further transform vitriolate of tartar.At present, the acquisition of high quality schoenite is mainly by two kinds of approach: the one, and the reaction of raw material mineral obtains the very high schoenite ore deposit of sodium chloride content, obtains higher-grade schoenite concentrate through operations such as flotation, washings again; The 2nd, obtain (as disclosed a kind of " method that cold process, hot legal system are got the higher-grade schoenite " in the Chinese patent " 88103389.8 ") by the thermosol cold crystallization.No matter which kind of method to obtain the high quality schoenite with, all need further react just with higher-grade Repone K and can obtain vitriolate of tartar.Produce vitriolate of tartar cost height with aforesaid method, low, the complex process of the utilization ratio of potassium and sulfate radical.
The objective of the invention is to provide a kind of quality that improves potassium product for fear of above-mentioned the deficiencies in the prior art part, improve potassium and sulfate radical utilization ratio, simplify the preparation method of the vitriolate of tartar of technological process.
Purpose of the present invention can realize by following measure:
A kind of preparation method of vitriolate of tartar is that carnallite and thenardite raw mineral materials are mixed with circulation schoenite mother liquor, potassium sulfate mother liquid; The mass ratio of potassium, magnesium, sulfate radical and water is 1 in the mixture: (0.50～0.84): (1.00～1.40): (9.00～14.00); Mixture is carried out the thermosol reaction under 50-69 ℃, reaction times is 15-60 minute, the liquid-solid mixed slurry that the reaction back forms, can obtain rubble salt and saturated solution through the insulation solid-liquid separation, after discarding rubble salt saturated solution is cooled to 0～19 ℃, crystallization goes out the mixture (being soft potassium mixed salt) of schoenite and Repone K, and solid-liquid separation gets soft potassium mixed salt and soft potassium mother liquor, and the mass ratio of schoenite and Repone K is (1.7-2.2) in the mixed salt: 1; Mixed salt is pressed (1.28-1.34): after 1 mass ratio adds the water reaction; Solid-liquid separation gets potassium sulfate mother liquid and vitriolate of tartar; The mother liquor that obtains in the said process can turn back to the thermosol step cycle and use.
Purpose of the present invention also can realize by following measure:
A kind of preparation method of vitriolate of tartar is that the optimum quality ratio of potassium, magnesium, sulfate radical and water in the mixture of carnallite and thenardite raw mineral materials and schoenite mother liquor, potassium sulfate mother liquid is 1: 0.70: 1.20: 11.00; The optimum temps of thermosol reaction is that 62 ℃, time are 30 minutes; When above-mentioned raw mineral materials was carnallite, potassium sulfate mother liquid also can remove to decompose carnallitite.
The present invention has following advantage compared to existing technology:
1, the mass ratio of potassium, magnesium, sulfate ion and the water in the mixture selected for use of the present invention is suitable, thereby the mixture that can obtain producing low schoenite of the required foreign matter content of vitriolate of tartar and Repone K after the reaction of thermosol, cold crystallization is suitable, do not need to add again refined potassium chloride, can directly make and extract high-quality vitriolate of tartar, reduced cost, simplify technological process.
2, soft potassium mother liquor and the potassium sulfate mother liquid that is produced in the process of the present invention can turn back to the thermosol operation, or potassium sulfate mother liquid turns back to the cold decomposition process of carnallite, improved the utilization ratio of potassium and sulfate radical.
3, the K of vitriolate of tartar of the present invention before not dry
2SO
4Content greater than 95%, the content of chlorine less than 1%, the content of water-insoluble is less than 0.1%.
The present invention also will be described in further detail in conjunction with the embodiments:
Embodiment one:
Certain salt lake brine Exposure to Sunlight gets carnallite, and the carnallite water decomposition is got sylvite, gets 107.0 parts of sylvites, wherein contains NaCl40.19%, KCl36.476, MgCl
28.01%, water-insoluble 0.61%, adds 39.3 parts of thenardites, wherein contains Na
2SO
491.16%, water-insoluble 6.71%; With above-mentioned two kinds of materials and 1000 parts of soft potassium mother liquors; And 117 parts of potassium sulfate mother liquids mix; The mass ratio of the potassium in the mixture, magnesium, sulfate radical and water is 1: 0.80: 1.30: 13.80, mix the back under 55 ℃ and agitation condition, and reacted 20 minutes, be incubated solid-liquid separation then and get rubble salt and saturated solution; Rubble salt is 92.4 parts, wherein contains NaCl81.34%, water-insoluble 3.98%; Separating obtained saturated solution is cooled to 6 ℃ under agitation condition, carry out solid-liquid separation and get soft potassium mixed salt and soft potassium mother liquor; Soft potassium mixed salt is 89.0 parts; The schoenite in the soft potassium mixed salt and the mass ratio of Repone K are 1.7: 1,1000 parts of molten step of reaction of returnable heat of the soft potassium mother liquor of gained.Above-mentioned soft potassium mixed salt is added 69.4 parts in water, and stirring reaction is 30 minutes under 55 ℃ of conditions, is cooled to 25 ℃ then and carries out solid-liquid separation, and 41.1 parts of the vitriolate of tartar of must wetting wherein contain K
2SO
495.36% (K
2O51.63%), Cl
-0.52%, water-insoluble 0.03%; Wet vitriolate of tartar drying gets potassium sulfate fertilizers; 117 parts of potassium sulfate mother liquids of gained return the thermosol step of reaction.
Embodiment two:
By 263 parts of 126 parts of cold decomposition carnallites of potassium sulfate mother liquid, divide to solve 170 parts of sylvites, wherein contain KCl35.71%, NaCl24.23%, MgCl
216.97%, water-insoluble 0.33%; Above-mentioned sylvite and 1000 parts of soft potassium mother liquors of 54.8 parts of gas of thenardite are mixed; The mass ratio of potassium, magnesium, sulfate radical and water is 1: 0.56: 1.10 in the mixture: 9.80; Mixture thermosol reaction 30 minutes under 68.9 ℃ and agitation condition gets rubble salt and saturated solution through the insulation solid-liquid separation then, and wherein rubble salt contains NaCl81.95%, water-insoluble 4.63%; Get rid of rubble salt; With saturated solution under agitation condition; Be cooled to 12 ℃ and carry out solid-liquid separation and get 1000 parts in 98.5 parts of soft potassium mixed salts and soft potassium mother liquor, soft potassium mother liquor returns the thermosol stage, and schoenite and Repone K mass ratio are 2.1: 1 in the soft potassium mixed salt; 98.5 parts of above-mentioned soft potassium mixed salts are added 73.6 parts of entry together make potassium sulphate fertilizer, wherein contain K with above-mentioned example
2SO
495.30% (K
2O51.59%), Cl
-0.47%, water-insoluble 0.08%; 126 parts of potassium sulfate mother liquids of gained remove cold decomposition carnallite.
Claims (3)
1, a kind of preparation method of vitriolate of tartar is characterized in that carnallite and thenardite raw mineral materials are mixed with circulation schoenite mother liquor, potassium sulfate mother liquid; The mass ratio of potassium, magnesium, sulfate radical and water is 1 in the mixture: (0.50～0.84): (1.00～1.40): (9.00～14.00); Mixture is carried out the thermosol reaction under 50-69 ℃, reaction times is 15-60 minute, the liquid-solid mixed slurry that the reaction back forms, can obtain rubble salt and saturated solution through the insulation solid-liquid separation, after discarding rubble salt saturated solution is cooled to 0～19 ℃, crystallization goes out the mixture (being soft potassium mixed salt) of schoenite and Repone K, and solid-liquid separation gets soft potassium mixed salt and soft potassium mother liquor, and the mass ratio of schoenite and Repone K is (1.7～2.2) in the mixed salt: 1; Mixed salt is pressed (1.28～1.34): after 1 mass ratio added the water reaction, solid-liquid separation got potassium sulfate mother liquid and vitriolate of tartar; The mother liquor that obtains in the said process can turn back to the thermosol step cycle and use.
2, the preparation method of a kind of vitriolate of tartar as claimed in claim 1 is characterized in that potassium, magnesium, sulfate radical and the water optimum quality ratio in the mixture of carnallite and thenardite raw mineral materials, schoenite mother liquor, potassium sulfate mother liquid is 1: 0.70: 1.20: 11.00; The optimum temps of thermosol reaction is that 62 ℃, time are 30 minutes.
3, the preparation method of a kind of vitriolate of tartar as claimed in claim 1 is characterized in that when above-mentioned raw mineral materials is carnallite potassium sulfate mother liquid also can remove to decompose carnallitite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93100790A CN1038833C (en) | 1993-01-08 | 1993-01-08 | Method for prepn. of potassium sulphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93100790A CN1038833C (en) | 1993-01-08 | 1993-01-08 | Method for prepn. of potassium sulphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1089576A CN1089576A (en) | 1994-07-20 |
| CN1038833C true CN1038833C (en) | 1998-06-24 |
Family
ID=4983230
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93100790A Expired - Fee Related CN1038833C (en) | 1993-01-08 | 1993-01-08 | Method for prepn. of potassium sulphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1038833C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100488874C (en) * | 2004-05-12 | 2009-05-20 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing potassium sulfate by using potassium mixed salt |
| CN103466662B (en) * | 2013-09-23 | 2015-04-01 | 河北工业大学 | Method for preparing potassium sulfate with large grain diameter by utilizing reaction crystallization |
| CN104016381A (en) * | 2014-05-31 | 2014-09-03 | 陈兆华 | Preparing method of picromerite by adopting mother liquor of potassium sulfate production by conversion method and sodium sulfate as raw materials |
| CN104529563A (en) * | 2014-11-20 | 2015-04-22 | 国投新疆罗布泊钾盐有限责任公司 | Method used for preparing potassium sulfate fertilizer from carnallite |
| CN104692420A (en) * | 2015-03-26 | 2015-06-10 | 茫崖兴元钾肥有限责任公司 | Potassium sulphate preparing method through thermal melting, refrigeration and double decomposition crystallization method |
| WO2017108876A1 (en) * | 2015-12-22 | 2017-06-29 | Yara Dallol Bv | Method for the control of sulphate forming compounds in the preparation of potassium sulphate from potassium-containing ores at high ambient temperatures |
| CN107827127A (en) * | 2017-12-04 | 2018-03-23 | 青海中航资源有限公司 | A kind of method that potassium sulfate Water soluble fertilizer is produced using low grade potassium ore deposit |
| 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 |
| CN113247920A (en) * | 2021-05-24 | 2021-08-13 | 青海联宇钾肥有限公司 | Method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US453336A (en) * | 1891-06-02 | Washing-machine | ||
| CN1037492A (en) * | 1988-05-12 | 1989-11-29 | 国家海洋局天津海水淡化与综合利用研究所 | The method for preparing vitriolate of tartar with mixing salt and Repone K |
-
1993
- 1993-01-08 CN CN93100790A patent/CN1038833C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US453336A (en) * | 1891-06-02 | Washing-machine | ||
| CN1037492A (en) * | 1988-05-12 | 1989-11-29 | 国家海洋局天津海水淡化与综合利用研究所 | The method for preparing vitriolate of tartar with mixing salt and Repone K |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1089576A (en) | 1994-07-20 |
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