CN1128760C - Method for preparing potassium sulfate by using sulfate type potassium-containing bittern - Google Patents
Method for preparing potassium sulfate by using sulfate type potassium-containing bittern Download PDFInfo
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- CN1128760C CN1128760C CN00112497A CN00112497A CN1128760C CN 1128760 C CN1128760 C CN 1128760C CN 00112497 A CN00112497 A CN 00112497A CN 00112497 A CN00112497 A CN 00112497A CN 1128760 C CN1128760 C CN 1128760C
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- potassium
- mixed salt
- sulfate
- magnesium mixed
- sodium chloride
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Abstract
The present invention relates to a method for preparing potassium sulfate from sulfate brine with potassium, which comprises the following steps that sulfate brine with potassium is sunned on a beach to prepare crude mixed salt of potassium and magnesium, the mixed salt of potassium and magnesium is pulverized and ground, saturated bittern of the mixed salt of potassium and magnesium is used for blending pulp, sodium chloride as an impurity is removed by a reverse flotation technology, and thus, the refined mixed salt of potassium and magnesium is obtained; the refined mixed salt of potassium and magnesium is mixed and reacts with potassium chloride and water to obtain picromerite which is mixed and reacts with the potassium chloride and the water to precipitate potassium sulfate. The present invention has the advantages that the method has simple process, the utilization rate of potassium ions and sulfate ions can be respectively improved to more than 70% and 65%, the sodium chloride obtained by reverse floatation technology can be used as an industrial salt so as to fully improve the utilization rate of bittern resource and not generate three wastes.
Description
The present invention relates to the method for a kind of preparation method of vitriolate of tartar, particularly preparing potassium sulfate by using sulfate type potassium-containing bittern.
In the prior art, United States Patent (USP) 3.589.871 (1971) discloses a kind of method of preparing potassium sulfate with sulfate type bittern.This method is regulated the bittern composition with vitriolate type bittern by converting halogen, removes part sodium-chlor, then makes kainite (KClMgSO salt Tanaka by the Exposure to Sunlight method
43H
2O), levigate after, with potassium sulfate mother liquid wash thick schoenite; Potassium content less than 8% low-grade sylvite magnesium alum through transforming, direct flotation gets thick kainite, thick schoenite with the potassium sulfate solution classification wash smart schoenite, smart schoenite adds Repone K and water under 55 ℃, classification is converted into the vitriolate of tartar slurry, after filtration, washing, drying make potassium product.The shortcoming of its existence is: this method kainite transforms to be needed to carry out in low mother liquid of magnesium, and potassium sulfate mother liquid configuration-system, complex technical process need be set separately; And owing to adopt direct floatation process, just kainite is carried out floatation recovery, be not fully used, cause the potassium ion (K of bittern resource and be present in the potassium and the sulfate radical composition that shine in the system mineral with other forms
+), sulfate ion (SO
4 2-) rate of recovery is low, potassium ion (K
+) rate of recovery can only reach about 60%,, sulfate ion (SO
4 2-) the ion rate of recovery can only reach about 50%.
The objective of the invention is at the prior art deficiency, proposed the reverse flotation of a kind of utilization, improve the method for the preparing potassium sulfate by using sulfate type potassium-containing bittern of potassium ion, the sulfate ion rate of recovery in the sulfate type potassium-containing halogen water resource sodium-chlor.
The objective of the invention is to be reached by following technical scheme, the present invention is a kind of method of preparing potassium sulfate by using sulfate type potassium-containing bittern, be characterized in that this method may further comprise the steps:
(a) sulfate type potassium-containing halogen water is shone through the beach, it is solid to separate the sodium-chlor of separating out earlier
Body shines the thick potassium magnesium that makes sodium chloride-containing (NaCl) 10-45% through continuing the beach
The mixed salt solid;
(b) the thick potassium magnesium mixed salt of sodium chloride-containing (NaCl) 10-45% is pulverized, levigate,
Saturated bittern with potassium magnesium mixed salt is sized mixing to the 20-40% concentration expressed in percentage by weight, adds
Go into the sodium-chlor flotation reagent, adopt reverse floatation process to slough impurity sodium-chlor
(NaCl), will slough slip behind the sodium-chlor again, make through dense, dehydration
Sodium-chlor (NaCl) content is less than 5% refining potassium magnesium mixed salt;
(c) less than 5% refining potassium magnesium mixed salt and purity not with sodium-chlor (NaCl) content
Be lower than 90% Repone K (KCl) and water under 10-60 ℃ of condition, by 1:
0.05-0.25: the effective ingredient weight ratio of 0.05-0.32 is mixed, through 0.5
Reaction in-3 hours separates one section conversion fluid, the schoenite that must separate out
(K
2SO
4MgSO
46H
2O) solid;
(d) with schoenite and Repone K (KCl), water under 10-70 ℃ of condition, press
1: 0.1-0.8: the effective ingredient weight ratio of 0.45-2.0 is mixed, through 0.25-3
Hour the reaction, separate two sections conversion fluids, the vitriolate of tartar solid that must separate out.
Wherein, the main component of the potassium magnesium mixed salt in above-mentioned (a) step comprises: vitriolate of tartar K
2SO
4, sal epsom MgSO
4, potassium chloride (KCl), sodium chloride nacl, magnesium chloride Mg Cl
2Combination cocrystallization body and mixture.In above-mentioned (c) step, refining potassium magnesium mixed salt system schoenite (K
2SO
4MgSO
46H
2O) principle is according to its phase region at five yuan of mutual system phase diagrams, adds Repone K (KCl) and water, is mixed in proportion, and is in order to make it put the crystallization phase region that is transferred to schoenite under this temperature mutually, to separate out the schoenite solid; And in above-mentioned (d) step, schoenite (K
2SO
4MgSO
46H
2O) principle of potassium sulfate making is according to its phase region at the mutual system of quadruplex phasor, adds Repone K (KCl) and water, is mixed in proportion, and is in order to make it put the crystallization phase region that is transferred to vitriolate of tartar under this temperature mutually, directly to separate out the vitriolate of tartar solid.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar, be characterized in shining in the thick potassium magnesium mixed salt solid process of system with the sulfate type potassium-containing halogen water beach, sulfate type potassium-containing halogen water shone through the beach to thick potassium magnesium mixed salt reach when saturated, separate the solid sodium chloride of separating out earlier again, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing (NaCl) 10-45% through continuing the beach.Make bittern in beach solarization process, the few as far as possible loss of potassium ion, sulfate ion, the best moment of as often as possible sloughing sodium-chlor again.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in making with extra care potassium magnesium mixed salt and produces in the process of schoenite, and temperature of reaction is 40 ℃, and the reaction times is 1 hour.This is the optimal reaction temperature and the optimum reacting time of this reaction process.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in making with extra care potassium magnesium mixed salt and produces in the process of schoenite, and the weight ratio of refining potassium magnesium mixed salt, Repone K, water is 1: 0.08-0.12: 0.16-0.24.This is the best proportioning of this reaction process.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in schoenite (K
2SO
4MgSO
46H
2O) two of potassium sulfate making sections conversion fluids make Repone K through evaporation.Change reaction conditions, make it put the crystallization phase region that is transferred at Repone K mutually, make precipitate high purity potassium chloride solid.Can return and be used for technology conversion reaction process of the present invention, also can be used as byproduct.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in refining potassium magnesium mixed salt system schoenite (K
2SO
4MgSO
46H
2O) one section conversion fluid returns this section conversion reaction or reverse flotation and takes off the sodium process and recycle.The one section conversion fluid is the saturated solution of schoenite.
The present invention does not compared with prior art need the mother liquor configuration-system is set separately, and technological process is simple; Owing to adopted reverse floatation process, the reverse flotation process is only sloughed impurity sodium-chlor, the potassium ion (K in the former bittern
+), sulfate ion (SO
4 2-) still be present in the refining potassium magnesium mixed salt after the flotation, finally be converted into vitriolate of tartar (K through two-step reaction
2SO
4) product, the potassium ion (K in the former bittern
+), sulfate ion (SO
4 2-) utilization ratio improves a lot, potassium ion (K wherein
+) utilization ratio can reach more than 70% sulfate ion (SO
4 2-) utilization ratio can reach more than 65%.And reverse flotation process gained tail salt sodium-chlor can be used as industrial salt and uses, and fully improved the resource utilization of bittern, no three wastes generation.
Accompanying drawing is technological process of production figure of the present invention.
Embodiment one.The following examples have further described summary of the invention of the present invention.In the present embodiment, sulfate type potassium-containing halogen water is selected East Platform Ji salt lake brine like this for use, teds the potassium magnesium mixed salt that makes through the salt pan, by weight composed as follows: K
+6.85%, SO
4 2-27.38%, Mg
2+5.89%, Cl
-7.91%, Na
+9.94%, H
2O32.03%.Potassium magnesium mixed salt is through pulverizing, levigate, make the material particular diameter behind the ore grinding account for weight percent 80% less than the content of 0.15 mm granules, size mixing to 25% concentration with saturated bittern then, with fatty amide as reverse floatation agent, carry out reverse flotation and take off sodium, to slough slip behind the sodium-chlor again through dense, dehydration, make refining potassium magnesium mixed salt, consist of by weight: K
+8.60%, SO
4 2-36.10%, Mg
2+7.84%, Cl
-6.24%, Na
+2.65%, H
2O39.40%.With purified potassium magnesium mixed salt and potassium chloride (KCl), water H
2O mixed by weight 1: 0.13: 0.16, and reaction is 0.5 hour under 40 ℃ of conditions, separates one section conversion fluid, the schoenite K that must separate out
2SO
4MgSO
46H
2The O solid consists of by weight: K
+16.45%, SO
4 2-40.16%, Mg
2+5.86%, Cl
-5.44%, Na
+2.33%, H
2O25.40%.Schoenite and potassium chloride (KCl), water H2O mixed by weight 1: 0.5: 1.1, and reaction is 1 hour under 60 ℃ of conditions, separates two sections conversion fluids, the vitriolate of tartar slurry of solids that must separate out, and after filtration, must potassium product after the drying, product purity reaches 98%.Two sections conversion fluids make high purity potassium chloride through evaporation.Potassium ion K in the whole technological process
+The rate of recovery reaches 78.75%, sulfate radical SO
4 2-The rate of recovery reaches 76.07%.
Embodiment two.The following examples continue to be described summary of the invention of the present invention, in the present embodiment, with the East Platform Ji like this salt lake brine be sulfate type potassium-containing halogen water, ted the potassium magnesium mixed salt of system through the salt pan, composed as follows by weight: K
+6.25%, SO
4 2-25.52%, Mg
2+6.53%, Cl
-17.60%, Na
+7.60%, H
2O32.03%.Potassium magnesium mixed salt is through pulverizing, levigate, make the material particular diameter behind the ore grinding account for weight percent 80% less than the content of 0.15 mm granules, size mixing to 20% concentration with saturated bittern then, with morpholine as reverse floatation agent, carry out reverse flotation and take off sodium, to slough slip behind the sodium-chlor again through dense, dehydration, make refining potassium magnesium mixed salt, consist of by weight: K
+8.15%, SO
4 2-35.30%, Mg
2+6.95%, Cl
-6.84%, Na
+2.21%, H
2O39.40%.With purified potassium magnesium mixed salt and potassium chloride (KCl), water H
2O mixed by weight 1: 0.05: 0.05, and reaction is 3 hours under 10 ℃ of conditions, separates one section conversion fluid, the schoenite K that must separate out
2SO
4MgSO
46H
2The O solid consists of by weight: K
+16.80%, SO
4 2-41.16%, Mg
2+5.72%, Cl
-5.14%, Na
+2.12%, H
2O29%.One section conversion fluid returns this section conversion reaction and recycles.Again with schoenite and potassium chloride (KCl), water H
2O mixed by weight 1: 0.1: 0.45, and reaction is 3 hours under 10 ℃ of conditions, separates two sections conversion fluids, the vitriolate of tartar solid phase prod that must separate out, and product purity reaches 98%.Two sections conversion fluids make Repone K through evaporation.The potassium ion K+ rate of recovery reaches 70.75% in the whole technological process, sulfate radical SO
4 2-The rate of recovery reaches 66.07%.
Embodiment three.The following examples continue to describe summary of the invention of the present invention, and in the present embodiment, East Platform Ji salt lake brine like this is a sulfate type potassium-containing halogen water, teds the potassium magnesium mixed salt of system through the salt pan, consists of by weight: K
+5.65%, SO
4 2-23.52%, Mg
2+5.53%, Cl
-15.60%, Na
+6.60%, H
2O43.1%.This potassium magnesium mixed salt is through pulverizing, levigate, make the material particular diameter behind the ore grinding account for weight percent 80% less than the content of 0.15 mm granules, size mixing to 40% concentration with saturated bittern then, with fatty amide as reverse floatation agent, carry out reverse flotation and take off sodium, to slough slip behind the sodium-chlor again through dense, dehydration, make refining potassium magnesium mixed salt, consist of by weight: K
+7.65%, SO
4 2-34.30%, Mg
2+6.55%, Cl
-5.48%, Na
+2.81%, H
2O38.01%.With purified potassium magnesium mixed salt and potassium chloride (KCl), water H
2O mixed by weight 1: 0.25: 0.32, and reaction is 0.5 hour under 60 ℃ of conditions, separates one section conversion fluid, the schoenite K that must separate out
2SO
4MgSO
46H
2The O solid consists of by weight: K
+15.20%, SO
4 2-40.16%, Mg
2+5.92%, Cl
-6.52%, Na
+2.48%, H
2O39.72%.One section conversion fluid returns reverse flotation and takes off the sodium process and recycle.Again with schoenite and potassium chloride (KCl), water H
2O mixed by weight 1: 0.8: 2.0, and reaction is 0.25 hour under 70 ℃ of conditions, separates two sections conversion fluids, and the vitriolate of tartar solid that must separate out gets potassium product after the drying, and product purity reaches 98%.Potassium ion K in the whole technological process
+The rate of recovery reaches 65.75%, sulfate radical SO
4 2-The rate of recovery reaches 60.07%.
Claims (6)
1, a kind of method of preparing potassium sulfate by using sulfate type potassium-containing bittern is characterized in that this method may further comprise the steps:
(a) sulfate type potassium-containing halogen water is shone through the beach, separate the solid sodium chloride of separating out earlier, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing NaCl 10-45% through continuing the beach;
(b) the thick potassium magnesium mixed salt of sodium chloride-containing NaCl 10-45% is pulverized, levigate, size mixing to the 20-40% concentration expressed in percentage by weight with the saturated bittern of potassium magnesium mixed salt, add the sodium-chlor flotation reagent, adopt reverse floatation process to slough the impurity sodium chloride nacl, to slough slip behind the sodium-chlor again through dense, dehydration, make sodium chloride nacl content less than 5% refining potassium magnesium mixed salt;
(c) sodium chloride nacl content is not less than 90% potassium chloride (KCl) and water under 10-60 ℃ of condition less than 5% refining potassium magnesium mixed salt and purity, by 1: the effective ingredient weight ratio of 0.05-0.25: 0.05-0.32 is mixed, through reaction in 0.5-3 hour, separate one section conversion fluid, the schoenite K that must separate out
2SO
4MgSO
46H
2The O solid;
(d) with schoenite and potassium chloride (KCl), water under 10-70 ℃ of condition, by 1: the effective ingredient weight ratio of 0.1-0.8: 0.45-2.0 is mixed, and through reaction in 0.25-3 hour, separates two sections conversion fluids, the vitriolate of tartar solid that must separate out.
2, the method for producing vitriolate of tartar according to claim 1, it is characterized in that shining in the thick potassium magnesium mixed salt solid process of system with the sulfate type potassium-containing halogen water beach, sulfate type potassium-containing halogen water shone through the beach to thick potassium magnesium mixed salt reach when saturated, separate the solid sodium chloride of separating out earlier again, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing NaCl 10-45% through continuing the beach.
3, the method for producing vitriolate of tartar according to claim 1, it is characterized in that refining potassium magnesium mixed salt produce schoenite process in, temperature of reaction is 40 ℃, the reaction times is 1 hour.
4, the method for producing vitriolate of tartar according to claim 1 is characterized in that making with extra care potassium magnesium mixed salt and produces in the process of schoenite, and the weight ratio of refining potassium magnesium mixed salt, Repone K, water is 1: 0.08-0.12: 0.16-0.24.
5, the method for producing vitriolate of tartar according to claim 1 is characterized in that schoenite K
2SO
4MgSO
46H
2Two sections conversion fluids of O potassium sulfate making make Repone K through evaporation.
6, the method for producing vitriolate of tartar according to claim 1 is characterized in that refining potassium magnesium mixed salt system schoenite K
2SO
4MgSO
46H
2One section conversion fluid of O returns this section conversion reaction or reverse flotation and takes off the sodium process and recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00112497A CN1128760C (en) | 2000-08-29 | 2000-08-29 | Method for preparing potassium sulfate by using sulfate type potassium-containing bittern |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00112497A CN1128760C (en) | 2000-08-29 | 2000-08-29 | Method for preparing potassium sulfate by using sulfate type potassium-containing bittern |
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| Publication Number | Publication Date |
|---|---|
| CN1281822A CN1281822A (en) | 2001-01-31 |
| CN1128760C true CN1128760C (en) | 2003-11-26 |
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|---|---|---|---|
| CN00112497A Expired - Lifetime CN1128760C (en) | 2000-08-29 | 2000-08-29 | Method for preparing potassium sulfate by using sulfate type potassium-containing bittern |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321893C (en) * | 2002-09-25 | 2007-06-20 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate |
| CA2552104C (en) * | 2003-12-31 | 2009-11-24 | Council Of Scientific And Industrial Research | Process for recovery of sulphate of potash |
| 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 |
| CN1810644B (en) * | 2006-02-11 | 2010-06-16 | 国投新疆罗布泊钾盐有限责任公司 | Improved process of preparing potassium sulfate with bittern containing potassium and magnesium sulfite |
| CN102744142A (en) * | 2012-07-18 | 2012-10-24 | 中蓝连海设计研究院 | Floatation medium and floatation method for potassium-containing sulfate floatation |
| KR101527140B1 (en) * | 2012-12-24 | 2015-06-10 | 주식회사 포스코 | Method for extraction of potassium from brine |
| 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 |
| CN105237049A (en) * | 2015-09-01 | 2016-01-13 | 格尔木康生钾业科技发展有限公司 | Production process of potassium sulfate specially used for drop irrigation |
| CN105967211B (en) * | 2016-05-08 | 2017-04-19 | 辽宁工程技术大学 | Method for preparing potassium sulfate from brine |
| CA3076265C (en) * | 2017-10-13 | 2021-05-25 | Novopro Projects Inc. | Systems and methods of producing potassium sulfate |
| CN115707656A (en) * | 2021-08-20 | 2023-02-21 | 中蓝连海设计研究院有限公司 | Method for extracting potassium sulfate from solar salt seawater |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1014818B (en) * | 1984-12-28 | 1991-11-20 | 富士重工业株式会社 | Fuel cock for an internal combustion engine |
| CN1076435A (en) * | 1992-03-13 | 1993-09-22 | 化学工业部化学矿产地质研究院 | Saltpan method is produced schoenite and vitriolate of tartar |
| CN1131639A (en) * | 1995-11-27 | 1996-09-25 | 中国科学院青海盐湖研究所 | Method for preparing potassium sulfate with sulfate type bittern |
-
2000
- 2000-08-29 CN CN00112497A patent/CN1128760C/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1014818B (en) * | 1984-12-28 | 1991-11-20 | 富士重工业株式会社 | Fuel cock for an internal combustion engine |
| CN1076435A (en) * | 1992-03-13 | 1993-09-22 | 化学工业部化学矿产地质研究院 | Saltpan method is produced schoenite and vitriolate of tartar |
| CN1131639A (en) * | 1995-11-27 | 1996-09-25 | 中国科学院青海盐湖研究所 | Method for preparing potassium sulfate with sulfate type bittern |
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| Publication number | Publication date |
|---|---|
| CN1281822A (en) | 2001-01-31 |
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