CN1220968A - Technology for preparation of potassium sulfate using potassium resource and magnesium resource and natural thenardite - Google Patents
Technology for preparation of potassium sulfate using potassium resource and magnesium resource and natural thenardite Download PDFInfo
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- CN1220968A CN1220968A CN 97123278 CN97123278A CN1220968A CN 1220968 A CN1220968 A CN 1220968A CN 97123278 CN97123278 CN 97123278 CN 97123278 A CN97123278 A CN 97123278A CN 1220968 A CN1220968 A CN 1220968A
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Abstract
A process for preparing potassium sulfate with potassium- and magnesium-containing resources and natural anhydrous mirabilite includes such technological steps as mixing the potassium- and magnesium-containing resources from salt lake and natural anhydrous mirabilitie with the mother liquid of mixed soft potassium salt, thermodissolving reaction, holding temp for a certain time, separating to obtain coarse soft halite and supernatant, mixing the supernatant with mother liquid of potassium sulfate, cooling, crystallizing mixed soft potassium salt, solid-liquid separation to obtain its mother liquid which is returned to thermodissolving step, adding water to mixed soft pottasium salt, converting to obtain potassium sulfate and mother liquid, and returning the mother liquid back to thermo-dissolving step. Its advantages are simple process and low cost.
Description
The present invention relates to field of inorganic chemical engineering, especially a kind of novel process of utilizing salt lake potassium resource and magnesium resource and thenardite to produce vitriolate of tartar.
With mineral be raw material produce vitriolate of tartar preferably technological process be to make high-quality schoenite earlier, further transform with high-quality Repone K then and make 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 high-quality schoenite with, all need further react just with higher-grade Repone K and can obtain vitriolate of tartar.These two kinds of methods are produced vitriolate of tartar cost height, and the utilization ratio of potassium and sulfate radical is low, complex process.At present, produce the best technology of vitriolate of tartar (as disclosed a kind of " utilizing salt pan carnallitite and thenardite to produce the method for vitriolate of tartar " in the Chinese patent " 8,710,339 34.8 ".This method is confined to carnallite and vitriolate of tartar is produced in the thenardite conversion reaction, and in the end remove to decompose carnallite with potassium sulfate mother liquid, soft potassium mother liquor is then more and more with the long-pending amount of cycle index, is the ratio of guaranteeing each ion in the dosing and the water concentrated soft potassium mother liquor that need consume energy.
The objective of the invention is for fear of above-mentioned the deficiencies in the prior art part, and provide a kind of quality that can improve potassium product, the utilization ratio that improves potassium and sulfate radical, technological process to simplify, raw material range is wide, the utilize potassium resource and magnesium resource and thenardite of the concentrated soft potassium mother liquor that need not to consume energy are produced the novel process of vitriolate of tartar.
Purpose of the present invention can realize by following measure:
A kind of novel process of utilizing potassium resource and magnesium resource and thenardite to produce vitriolate of tartar, comprise following processing step: (1) is got potassium resource ore deposit, magnesium resource, thenardite and is mixed with circulation soft potassium mixed salt mother liquor, and the mass ratio of potassium, magnesium, sulfate radical and water is 1 in the mixture: (0.5-0.8): (1-1.5): (9-1 5); Mixture is carried out the thermosol reaction under 50-100 ℃, the reaction times is 15-60 minute, gets solid-liquid compound oar after the reaction, separates to get rubble salt and thermosol clear liquid through the solid-liquid insulation; (2) the thermosol clear liquid is cooled to 0-10 ℃, the mixture (being soft potassium mixed salt) of schoenite and Repone K is separated out in crystallization, and solid-liquid separation gets soft potassium mixed salt and soft potassium mixed salt mother liquor, the soft potassium mixed salt mother liquor is back to the thermosol step cycle uses; The mass ratio of schoenite and Repone K is (1.7-2.2) in the mixed salt: 1; (3) with soft potassium mixed salt by (1.2-1.3): 1 mass ratio add water react vitriolate of tartar and potassium sulfate mother liquid; Described potassium resource ore deposit can be carnallitite, sylvite, thick potash fertilizer, potassium magnesium mixed salt, kainite, leonite, glaserite ore deposit class resource; Described magnesium resource can be carnallitite, sal epsom, magnesium chloride and magniferous old bittern class resource; Other potassium sulfate mother liquid of gained in described technology (3) goes on foot is back in (2) step process and mixes with the thermosol clear liquid, and the weight of pressing the 9-14% of thermosol clear liquid adds potassium sulfate mother liquid.
The present invention has following advantage compared to existing technology:
1, the present invention selects for use and contains potassium resource, magnesium resource and soft potassium mixed salt mother liquor and be mixed together, the mass ratio of potassium, magnesium, sulfate radical and water is suitable in the mixture, can obtain producing the required intermediate raw material of vitriolate of tartar after the reaction of thermosol, cold crystallization, this raw material is impure low and ratio schoenite and Repone K is suitable; Need not add high-quality Repone K and can make high-quality vitriolate of tartar, reduce cost, simplify technological process.
2, the soft potassium mixed salt mother liquor that is produced in the technological process of the present invention turns back to the thermosol burden process, potassium sulfate mother liquid returns to be allocated in the thermosol clear liquid by a certain percentage, recycle, improved the utilization ratio of potassium and sulfate radical, avoided potassium sulfate mother liquid to be back to the thermosol step of reaction and caused the mother liquor accumulation too much to need the spissated shortcoming of power consumption; Needing when the thermosol clear liquid cools off in the similar technology to have avoided the defective of water distribution simultaneously.
3, the raw material that uses in the technology of the present invention (containing magnesium resource, potassium resource and thenardite) scope is wide, and the grade of mineral wealth is not had strict demand.
4, vitriolate of tartar quality of the present invention is greater than 95%, and chloride ion content is less than 1.0%, and water insoluble matter content is less than 0.1%.
The present invention also will be described in further detail in conjunction with the embodiments:
Embodiment one:
210 parts (wherein sodium chloride-containing 63.14% to get sylvite, Repone K 28.98%, water-insoluble 2.88%), 79.7 parts (wherein contains sodium sulfate 85.0% to add thenardite, sodium-chlor 1.0%, calcium sulfate 4.0%, water-insoluble 5.0%), add 47.4 parts of magnesium chloride hexahydrates (wherein containing magnesium chloride 46.82%), mix with 1000 parts soft potassium mixed salt mother liquor; The mass ratio of potassium, magnesium, sulfate radical and water in the mixture was controlled at 1: 0.69: 1.47: 12; The temperature of thermosol reaction is controlled at 62 ℃, and the reaction times was controlled at 30 minutes, is incubated solid-liquid separation after reaction is finished and gets rubble salt and thermosol clear liquid, gets 216.83 parts of rubble salt (wherein sodium chloride-containing 89.64%, water-insoluble 4.15%); Allocate potassium sulfate mother liquid into by 12.0% of thermosol clear liquid, mixed solution under agitation is cooled to 5 ℃, carries out solid-liquid separation and gets 123.23 parts of soft potassium mixed salts and soft potassium mixed salt mother liquor 1109.04; Schoenite in the soft potassium mixed salt and Repone K mass ratio are 1.86: 1, and the soft potassium mother liquor of gained returns the thermosol batching; Above-mentioned soft potassium mixed salt is added 98.58 parts of entry, stirring reaction is 30 minutes under 55 ℃ of conditions, be cooled to 25 ℃ then, carry out solid-liquid separation and must wet that 63.86 parts { wherein vitriolate of tartar contained for 95.06% (being equivalent to contain potassium oxide 51.39%) to vitriolate of tartar, chlorion 0.35%, water-insoluble 0.03%}, wet vitriolate of tartar drying gets potassium product; Resulting 163.89 parts potassium sulfate mother liquid turns back in the thermosol clear liquid.
Embodiment two:
Get thick potash fertilizer and (wherein contain Repone K 60.90% for 99.94 parts, magnesium chloride 2.98%, calcium sulfate 2.63%, sodium-chlor 33.61%, water-insoluble 2.20%), 51.71 parts (wherein contains sodium sulfate 85.0% to add thenardite, sodium-chlor 1.0%, calcium sulfate 4.0%, water-insoluble 5.0%), add 41.28 parts of magnesium sulfate heptahydrates (wherein sulfur acid magnesium 48.82%); The soft potassium mixed salt mother liquor of above-mentioned three kinds of raw materials with 1000 parts mixed; The mass ratio of potassium, magnesium, sulfate radical and water in the mixture was controlled at 10.69: 1.45: 11; Mixture stirring reaction 30 minutes under 70 ℃ of conditions, be incubated after reaction is finished separate rubble salt and thermosol clear liquid, 85.19 parts of rubble salt (wherein sodium chloride-containing 89.64%, water-insoluble 5.75%); The thermosol clear liquid adds 10% potassium sulfate mother liquid, is cooled to 7 ℃ under agitation condition, carries out solid-liquid separation and gets 1096.66 parts in 121.85 parts of soft potassium mixed salts and soft potassium mixed salt mother liquor; The soft potassium mother liquor of gained is returned the thermosol batching; Above-mentioned soft potassium mixed salt is added 97.48 parts of entry, and { wherein vitriolate of tartar contains 96.98% (being equivalent to contain potassium oxide 52.42%), chlorion 0.45%, water-insoluble 0.04%} together to make 57.27 parts of vitriolate of tartar with example; Resulting 162.06 parts of potassium sulfate mother liquids turn back in the thermosol clear liquid.
Embodiment three:
Get 104 parts in thick potash fertilizer and (wherein contain Repone K 47.67%, magnesium chloride 2.98%, calcium sulfate 2.63%, sodium-chlor 36.84%, water-insoluble 2.20%), 65.4 parts (wherein contains sodium sulfate 85.0% to add thenardite, sodium-chlor 1.0%, calcium sulfate 4.0%, water-insoluble 5.0%), 23.29 parts (wherein sodium chloride-containing 0.38% for magniferous old bittern, Repone K 0.1%, calcium sulfate 0.01%, sal epsom 1.88%, magnesium chloride 32.81%); The soft potassium mixed salt mother liquor of above-mentioned three kinds of raw materials with 1000 parts mixed; The mass ratio of potassium, magnesium, sulfate radical and water is 1: 0.63: 1.42 in the mixture: 12.5; Mixture stirring reaction 30 minutes under 65 ℃ of conditions is incubated solid-liquid separation after reaction is finished and gets rubble salt and thermosol clear liquid, wherein 114.0 parts of rubble salt (wherein sodium chloride-containing 87.05%, water-insoluble 6.20%); The thermosol clear liquid adds 10% potassium sulfate mother liquid, is cooled to 7 ℃ under agitation condition, carries out solid-liquid separation and gets soft potassium mixed salt and soft potassium mixed salt mother liquor, and wherein 118.6 parts of soft potassium mixed salts and soft potassium mixed salt mother liquor are 1070.1 parts; The soft potassium mother liquor of gained is returned the thermosol batching; Above-mentioned soft potassium mixed salt is added 93.2 parts of entry, and { wherein vitriolate of tartar contains 95.67% (being equivalent to contain potassium oxide 51.72%), chlorion 0.66%, water-insoluble 0.03%} together to make vitriolate of tartar with example; Resulting 156.06 parts of potassium sulfate mother liquids turn back in the thermosol clear liquid.
Embodiment four:
Get thick potash fertilizer and (wherein contain Repone K 60.90% for 85.79 parts, magnesium chloride 2.98%, calcium sulfate 2.63%, sodium-chlor 36.61%, water-insoluble 2.20%), 37.65 parts (wherein contains sodium sulfate 85.0%, sodium-chlor 1.0%, calcium sulfate 4.0% to add thenardite, water-insoluble 5.0%), 62.56 parts (wherein sodium chloride-containing 13.80%, Repone K 13.78%, sal epsom 16.19% for potassium magnesium mixed salt, magnesium chloride 17.42%, lithium chloride 0.13%, water-insoluble 1.0%), the soft potassium mixed salt mother liquor of above-mentioned three kinds of raw materials with 1000 parts mixed; The mass ratio of potassium, magnesium, sulfate radical and water is 1: 0.68: 1.46 in the mixture: 12; Mixture stirring reaction 30 minutes under 65 ℃ of conditions is incubated solid-liquid separation after reaction is finished and gets rubble salt and thermosol clear liquid, wherein 65.38 parts of rubble salt (wherein sodium chloride-containing 88.29%, water-insoluble 6.10%); The thermosol clear liquid adds 10% potassium sulfate mother liquid, is cooled to 3.5 ℃ under agitation condition, carries out solid-liquid separation and gets soft potassium mixed salt and soft potassium mixed salt mother liquor, and wherein 123.27 parts of soft potassium mixed salts and soft potassium mixed salt mother liquor are 1109.41 parts; The soft potassium mother liquor of gained is returned the thermosol batching; Above-mentioned soft potassium mixed salt is added 98.62 parts of entry, and { wherein vitriolate of tartar contains 95.83% (being equivalent to contain potassium oxide 51.80%), chlorion 0.72%, water-insoluble 0.05%} together to make vitriolate of tartar with example; Resulting 163.95 parts of potassium sulfate mother liquids turn back in the thermosol clear liquid.
Claims (1)
1, a kind of novel process of utilizing potassium resource and magnesium resource and thenardite to produce vitriolate of tartar, comprise following processing step: (1) is got potassium resource ore deposit, magnesium resource, thenardite and is mixed with circulation soft potassium mixed salt mother liquor, and the mass ratio of potassium, magnesium, sulfate radical and water is 1 in the mixture: (0.5-0.8): (1-1.5): (9-15); Mixture is carried out the thermosol reaction under 50-100 ℃, the reaction times is 15-60 minute, gets solid-liquid compound oar after the reaction, separates to get rubble salt and thermosol clear liquid through the solid-liquid insulation; (2) the thermosol clear liquid is cooled to 0-10 ℃, the mixture (being soft potassium mixed salt) of schoenite and Repone K is separated out in crystallization, and solid-liquid separation gets soft potassium mixed salt and soft potassium mixed salt mother liquor, the soft potassium mixed salt mother liquor is back to the thermosol step cycle uses; The mass ratio of schoenite and Repone K is (1.7-2.2) in the mixed salt: 1; (3) with soft potassium mixed salt by (1.2-1.3): 1 mass ratio add water react vitriolate of tartar and potassium sulfate mother liquid; It is characterized in that described potassium resource ore deposit can be carnallitite, sylvite, thick potash fertilizer, potassium magnesium mixed salt, kainite, leonite, glaserite ore deposit class resource; Described magnesium resource can be carnallitite, sal epsom, magnesium chloride and magniferous old bittern class resource; Other potassium sulfate mother liquid of gained in described technology (3) goes on foot is back in (2) step process and mixes with the thermosol clear liquid, and the weight of pressing the 9-14% of thermosol clear liquid adds potassium sulfate mother liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 97123278 CN1220968A (en) | 1997-12-22 | 1997-12-22 | Technology for preparation of potassium sulfate using potassium resource and magnesium resource and natural thenardite |
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| CN 97123278 CN1220968A (en) | 1997-12-22 | 1997-12-22 | Technology for preparation of potassium sulfate using potassium resource and magnesium resource and natural thenardite |
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| CN1220968A true CN1220968A (en) | 1999-06-30 |
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| CN 97123278 Pending CN1220968A (en) | 1997-12-22 | 1997-12-22 | Technology for preparation of potassium sulfate using potassium resource and magnesium resource and natural thenardite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108349743A (en) * | 2015-05-08 | 2018-07-31 | 雅拉达洛尔有限公司 | The method that potassium sulfate is produced by phosphate-containing ore at a high ambient temperature |
-
1997
- 1997-12-22 CN CN 97123278 patent/CN1220968A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108349743A (en) * | 2015-05-08 | 2018-07-31 | 雅拉达洛尔有限公司 | The method that potassium sulfate is produced by phosphate-containing ore at a high ambient temperature |
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