CN1696059A - Method for preparing potassium sulfate by using potassium mixed salt - Google Patents
Method for preparing potassium sulfate by using potassium mixed salt Download PDFInfo
- Publication number
- CN1696059A CN1696059A CN 200410038989 CN200410038989A CN1696059A CN 1696059 A CN1696059 A CN 1696059A CN 200410038989 CN200410038989 CN 200410038989 CN 200410038989 A CN200410038989 A CN 200410038989A CN 1696059 A CN1696059 A CN 1696059A
- Authority
- CN
- China
- Prior art keywords
- schoenite
- raw material
- mother liquor
- conversion
- tartar
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 20
- 150000003839 salts Chemical class 0.000 title claims description 21
- 229910052700 potassium Inorganic materials 0.000 title claims description 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims description 16
- 239000011591 potassium Substances 0.000 title claims description 16
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title abstract description 4
- 229910052939 potassium sulfate Inorganic materials 0.000 title abstract description 4
- 235000011151 potassium sulphates Nutrition 0.000 title abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000012452 mother liquor Substances 0.000 claims abstract description 13
- 239000013505 freshwater Substances 0.000 claims abstract description 12
- 208000006558 Dental Calculus Diseases 0.000 claims description 16
- GMLLYEDWRJDBIT-UHFFFAOYSA-J magnesium;dipotassium;disulfate Chemical compound [Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GMLLYEDWRJDBIT-UHFFFAOYSA-J 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 abstract 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 5
- 241001131796 Botaurus stellaris Species 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- ILRLTAZWFOQHRT-UHFFFAOYSA-N potassium;sulfuric acid Chemical compound [K].OS(O)(=O)=O ILRLTAZWFOQHRT-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- SWHAQEYMVUEVNF-UHFFFAOYSA-N magnesium potassium Chemical compound [Mg].[K] SWHAQEYMVUEVNF-UHFFFAOYSA-N 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
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Abstract
The invention discloses a method for preparing potassium sulfate by using mixed potassium salt, brackish water or fresh water as raw materials, in particular to a method for preparing potassium sulfate by converting a single mixed potassium salt raw material into picromerite and then converting the picromerite serving as a raw material. The method has the characteristics of single raw material, short process flow, simple equipment, easy operation, low investment, recyclable conversion mother liquor, no generation of three wastes and the like.
Description
The present invention relates to a kind of method of producing vitriolate of tartar, particularly be reacted into schoenite, after transforming, produce the method for vitriolate of tartar again with single potassium mixed salt feedstock conversion.
In the prior art, CN1044108C discloses a kind of novel process of preparing potassium sulfate with sulfate type bittern, this invention is vitriolate type bittern to be shone in the salt pan make potassium magnesium mixed salt, with this raw material at normal temperatures decomposition and inversion obtain the mixing salt of Repone K and schoenite, the further decomposition and inversion of this mixing salt is produced vitriolate of tartar; CN1281822A, the CN1439602A patent of invention is disclosed to be produced in the method for vitriolate of tartar, except that having adopted the medicament flotation, in the conversion reaction of schoenite, has adopted the operation steps that adds Repone K.
The objective of the invention is at the deficiencies in the prior art, invented and a kind ofly used single potassium mixed salt raw material to produce the method for vitriolate of tartar.
The present invention adopts artificial beach, salt pan, area, salt lake to shine the potassium mixed salt that obtains to be raw material, under differing temps, to produce vitriolate of tartar by two sections conversion methods.It is characterized by: potassium mixed salt raw material does not promptly produce Repone K when differing temps transforms, need not add Repone K yet, just can directly produce vitriolate of tartar, the mother liquor E of the course of processing
1, E
2Reusable edible only uses slightly salty or fresh water, and therefore, the present invention has that raw material is single, technical process is short, equipment is simple, easy to operate, less investment, has made full use of advantages such as salt lake resources and envrionment conditions; The course of processing does not have three wastes generation, free from environmental pollution.
The present invention realizes as follows:
1, potassium mixed salt is by weight composed as follows: K
1+8.00～11.00%, Mg
2+6.50～8.50%, Na
1+5.00～8.00%, SO
4 2-15.00～25.00%, Cl
1-25.00～30.00%, H
2O 25.00～40.00%, add E
2Mother liquor and salinity are carried out one section conversion reaction at slightly salty or the fresh water of 6～9g/l under 20～35 ℃ of agitation conditions, solid-liquid separation obtains the solid schoenite, and its weight ratio is composed as follows: K
1+18.00～19.00%, Mg
2+5.50～6.50%, Na
1+0.20～1.00%, SO
4 2-43.00～45.00%, Cl
1-1.00～2.00%, the E after the separation
1Mother liquor enters the salt pan, recycles.
2, aforesaid schoenite joins in two sections conversion tanks, adds hot slightly salty or hot fresh water and carry out two sections conversion reactions under 55～65 ℃ of agitation conditions, carries out solid-liquid separation, E after the conversion fully
2Mother liquor joins in one section conversion and utilizes, and solid is the wet basis vitriolate of tartar, promptly gets potassium product after drying.
In the above-mentioned steps 1, be aforementioned potassium mixed salt wherein, E
2The slightly salty of mother liquor and adding or fresh water put according to K conversion reaction according to its certain proportion allotment mutually
1+, Na
1+, Mg
2+//Cl
1-, SO
4 2--H
2Five yuan of salt-water system phasors of O move in the crystallization phase region of schoenite under this temperature, and crystalline solid is schoenite.
In the above-mentioned steps 2, the principle that schoenite is produced vitriolate of tartar is according to K
1+, Mg
2+//Cl
1-, SO
4 2--H
255 ℃ of phasors of O quaternary salt-water system move in the crystallizing field of vitriolate of tartar under this temperature conversion reaction, obtain solid sulphuric acid potassium.
Technology of the present invention can further realize by following scheme.The aforementioned method of producing vitriolate of tartar is characterized in potassium mixed salt raw material, E
2Mother liquor, slightly salty or fresh water is by weight: 1: 1.0～1.5: 0.2～0.5 mixes, under 20～35 ℃ of agitation conditions, and conversion reaction 0.5～1.5 hour, this is the best proportioning and the reaction conditions of one section conversion reaction process.
Technology of the present invention can also further realize by following scheme.The aforementioned method of producing vitriolate of tartar, be characterized in the solid schoenite, hot slightly salty or hot fresh water by weight: 1: 1.0～1.5 mix, under 55～65 ℃ of agitation conditions, conversion reaction 0.5～1.5 hour, this is the best proportioning and the reaction conditions of two sections conversion reaction processes.
The present invention has finished laboratory experiment and has produced 500 tons pilot plant test per year in November, 2002～2003 year October in the salt lake, Lop Nur.The following examples have further been set forth summary of the invention of the present invention.
In the present embodiment, be to shine the potassium mixed salt that obtains on artificial beach, salt pan, by weight composed as follows: K with Lop Nur magnesium sulfate bittern
1+9.20%, Mg
2+7.21%, Na
1+7.98%, SO
4 2-21.42%, Cl
1-25.87%, H
2O 28.10%, with E
2Mother liquor, slightly salty or fresh water 1: 1.0～1.5: 0.2～0.5 are deployed into slip by weight, and conversion reaction is 0.5～1.5 hour under 20～35 ℃ of agitation conditions, and solid-liquid separation obtains the solid schoenite; Again with this schoenite and hot slightly salty or hot fresh water by weight: 1: 1.0～1.5 are deployed into slip, conversion reaction is 0.5～1.5 hour under 55～65 ℃ of agitation conditions, separates two sections and transforms mother liquor, obtains solid sulphuric acid potassium, be potassium product after drying, product purity reaches K
1+39.85%, SO
4 2-52.96%, Cl
1-0.18%, K
2O content is 50.27%, quality product meets GB top grade product standard, single cycle potassium yield is 40.0～45.0%, potassium mixed salt raw material does not promptly produce Repone K in the whole course of processing, need not add Repone K yet, therefore, the present invention provides a kind of novel method for magnesium sulfate bittern exploitation and utilization of salt lake resources.
Process flow sheet is seen Figure of description.
Claims (3)
1, be raw material with potassium mixed salt, slightly salty or fresh water, under condition of different temperatures, directly produce the method for vitriolate of tartar by twice conversion, it is characterized in that, with above-mentioned raw materials under 20～35 ℃ of conditions by being converted into the solid schoenite, be raw material again with the schoenite, under 55～65 ℃ of conditions, obtain vitriolate of tartar by conversion.
2, by the described method of claim 1, it is characterized in that potassium mixed salt raw material, E
2Mother liquor, slightly salty or fresh water 1: 1.0～1.5: 0.2～0.5 are deployed into slip by weight, join in one section conversion tank, stir under 20～35 ℃ of conditions then and transform 0.5～1.5 hour; Solid-liquid separation obtains solid schoenite and E
1Mother liquor, E
1Mother liquor is sent into the salt pan, recycles.
3, by claim 1,2 described methods, it is characterized in that, single schoenite and hot slightly salty or hot fresh water mix according to 1: 1.0～1.5 weight ratio, join in two sections conversion tanks, under 55～65 ℃ of agitation conditions, through conversion reaction in 0.5～1.5 hour, directly obtain vitriolate of tartar, E after the solid-liquid separation
2Mother liquor returns preceding operation recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100389891A CN100488874C (en) | 2004-05-12 | 2004-05-12 | Method for preparing potassium sulfate by using potassium mixed salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100389891A CN100488874C (en) | 2004-05-12 | 2004-05-12 | Method for preparing potassium sulfate by using potassium mixed salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1696059A true CN1696059A (en) | 2005-11-16 |
| CN100488874C CN100488874C (en) | 2009-05-20 |
Family
ID=35348974
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100389891A Expired - Lifetime CN100488874C (en) | 2004-05-12 | 2004-05-12 | Method for preparing potassium sulfate by using potassium mixed salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100488874C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1810730B (en) * | 2006-02-11 | 2010-12-01 | 国投新疆罗布泊钾盐有限责任公司 | Improved process of preparing magnesium potassium sulfate fertilizer with bittern containing potassium and magnesium sulfite |
| CN1810729B (en) * | 2006-02-11 | 2011-04-27 | 国投新疆罗布泊钾盐有限责任公司 | Process of preparing magnesium potassium sulfate fertilizer with bittern potassium containing magnesium sulfite |
| CN102674405A (en) * | 2012-05-30 | 2012-09-19 | 河北工业大学 | Method for preparing potassium sulfate by using picromerite |
| CN107324849A (en) * | 2017-08-31 | 2017-11-07 | 化工部长沙设计研究院 | A kind of method for preparing potash magnesium sulphate fertilizer |
| CN107382381A (en) * | 2017-08-31 | 2017-11-24 | 化工部长沙设计研究院 | A kind of production technology of high-quality potash magnesium sulphate fertilizer |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2523114A1 (en) * | 1982-03-11 | 1983-09-16 | Alsace Mines Potasse | PROCESS FOR PRODUCING POTASSIUM SULFATE FROM SOLUTIONS CONTAINING MAGNESIUM CHLORIDE AND POTASSIUM CHLORIDE |
| CN1038833C (en) * | 1993-01-08 | 1998-06-24 | 中国科学院青海盐湖研究所 | Method for prepn. of potassium sulphate |
| CN1044108C (en) * | 1995-11-27 | 1999-07-14 | 中国科学院青海盐湖研究所 | Method for preparing potassium sulfate with sulfate type bittern |
| US6334990B1 (en) * | 1999-10-21 | 2002-01-01 | Airborne Industrial Minerals Inc. | Formulation of potassium sulfate, sodium carbonate and sodium bicarbonate from potash brine |
| CN1128760C (en) * | 2000-08-29 | 2003-11-26 | 化学工业部连云港设计研究院 | Method for preparing potassium sulfate by using sulfate type potassium-containing bittern |
| 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 |
-
2004
- 2004-05-12 CN CNB2004100389891A patent/CN100488874C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1810730B (en) * | 2006-02-11 | 2010-12-01 | 国投新疆罗布泊钾盐有限责任公司 | Improved process of preparing magnesium potassium sulfate fertilizer with bittern containing potassium and magnesium sulfite |
| CN1810729B (en) * | 2006-02-11 | 2011-04-27 | 国投新疆罗布泊钾盐有限责任公司 | Process of preparing magnesium potassium sulfate fertilizer with bittern potassium containing magnesium sulfite |
| CN102674405A (en) * | 2012-05-30 | 2012-09-19 | 河北工业大学 | Method for preparing potassium sulfate by using picromerite |
| CN102674405B (en) * | 2012-05-30 | 2014-03-19 | 河北工业大学 | Method for preparing potassium sulfate by using picromerite |
| CN107324849A (en) * | 2017-08-31 | 2017-11-07 | 化工部长沙设计研究院 | A kind of method for preparing potash magnesium sulphate fertilizer |
| CN107382381A (en) * | 2017-08-31 | 2017-11-24 | 化工部长沙设计研究院 | A kind of production technology of high-quality potash magnesium sulphate fertilizer |
| CN107324849B (en) * | 2017-08-31 | 2020-09-15 | 化工部长沙设计研究院 | Method for preparing potash magnesium sulphate fertilizer |
| CN107382381B (en) * | 2017-08-31 | 2020-09-15 | 化工部长沙设计研究院 | Production process of high-quality potassium magnesium sulfate fertilizer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100488874C (en) | 2009-05-20 |
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Addressee: Yuan Xuedong Document name: patent for invention |
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Granted publication date: 20090520 |
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