CN1131639A - Method for preparing potassium sulfate with sulfate type bittern - Google Patents
Method for preparing potassium sulfate with sulfate type bittern Download PDFInfo
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- CN1131639A CN1131639A CN 95120053 CN95120053A CN1131639A CN 1131639 A CN1131639 A CN 1131639A CN 95120053 CN95120053 CN 95120053 CN 95120053 A CN95120053 A CN 95120053A CN 1131639 A CN1131639 A CN 1131639A
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- bittern
- inversion
- potassium
- decomposition
- mixed salt
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Abstract
A process for preparing potassium sulfate from sulfate-type bittern includes such steps as evaporating in the sun to make mixed K-Mg salts by Na pool, bittern mingling pool and mixed K-Mg pool, decomposing and transforming at 10-25 deg.C, filtering, decomposing and transforming again at 45-60 deg.C, filtering, washing and drying, and features high yield, low comsumption of fresh water, low cost and recovery of mother liquor.
Description
The invention belongs to the salt-water system separation technology field, particularly a kind of method with preparing potassium sulfate with sulfate type bittern.
The existing method of producing vitriolate of tartar from vitriolate type bittern has: 1, United States Patent (USP) 3.589.871 (1971), this method is with sulfate type salt lake bittern, form by regulating bittern, adopt the mode of Exposure to Sunlight to make kainite in the salt pan, kainite is after levigate, again with potassium sulfate mother liquid wash thick soft potassium magnesium vanadium, low-grade kainite is through transforming, flotation gets thick schoenite, thick schoenite with the potassium sulfate mother liquid classification wash smart schoenite, smart schoenite adds KCl and water is the vitriolate of tartar slurry 55 ℃ of following decomposition and inversion, after filtration, washing, operations such as drying make potassium product.This method only is applicable to the area that temperature is higher, and has complex procedures, needs flotation reagent, defectives such as contaminate environment.
2, the application number by the application of Chinese Academy of Sciences Qinghai salt lake institute is 87103934, be to utilize sulfate type salt lake bittern to produce the technology of vitriolate of tartar, this technology be with potassium magnesium mixed salt ore deposit complete molten after, get the mixture of smart schoenite and Repone K in the salt pan Exposure to Sunlight, the transformation efficiency of single potassium is more than 50%, and then add Repone K and fresh water, get 55 ℃ of following decomposition and inversion that the vitriolate of tartar slip filters, washs, drying must potassium product.The weak point of this method is that the production cycle is long, and fresh water dosage is big, and single potassium transformation efficiency is low, and potassium sulfate mother liquid is recycle not.
The objective of the invention is shortcoming at the prior art existence, design a kind of novel process with preparing potassium sulfate with sulfate type bittern, this technology is not subjected to the temperature condition effect, it is simple to have operation, does not need flotation reagent, potassium single rate of recovery height, fresh water dosage is few, many advantages such as energy consumption is little, and production cost hangs down the potassium sulfate mother liquid reusable edible, and is free from environmental pollution.
This invention realizes by following technical scheme: (1) technical process is: system potassium magnesium mixed salt → decomposition and inversion one → filtration → decomposition and inversion two → filtration washing → dry packing → potassium product is shone in the salt pan.(2) processing condition are: the salt pan is shone system potassium magnesium mixed salt operation and is divided into the sodium pond, the system step is shone in three in bittern-mixing pool and potassium magnesium mixed salt pond etc., former halogen evaporation removes and anhydrates and sodium-chlor in the sodium pond, bittern enters bittern-mixing pool when saturated to vitriol, the saturated halogen that adds magnesium chloride in the bittern-mixing pool is regulated the composition of bittern, convert halogen ratio=bittern: the saturated halogen of magnesium chloride=1: 0.1～0.8 (ratio of volume), evaporation removes and anhydrates and sodium-chlor in the bittern-mixing pool, epsom salt, bittern enters potassium magnesium mixed salt pond when saturated to carnallitite, evaporation is anhydrated and is separated out potassium magnesium mixed salt in the potassium magnesium mixed salt pond, after the saturation point of magnesium chloride, carry out solid-liquid separation, part bittern is used to convert halogen, and Gu Kuang enters down operation: the invert point of decomposition and inversion one operation is that 10～25 ℃ of fresh water of 45～100% that add wet ore deposits amount are to potassium magnesium mixed salt decomposition and inversion; The invert point of decomposition and inversion two operations is 45～60 ℃, and 55～130% the fresh water that adds wet ore deposit amount is to schoenite and Repone K decomposition and inversion.In order to make the mother liquor recovery free from environmental pollution and abundant after the filtration, preferably a step mother liquor is entered and convert in the pond, two step mother liquors are sent into decomposition and inversion one in-process remove decomposition and inversion potassium magnesium mixed salt.One step mother liquor belongs to and contains potassium bittern, and two step mother liquors are filtration, washings, and two step mother liquors are sent into the rate of recovery that decomposition and inversion one operation can effectively improve vitriolate of tartar.The salt pan is shone system potassium magnesium mixed salt operation and is finished with sodium pond, bittern-mixing pool, potassium magnesium mixed salt pond three solarization systems step, sodium pond and bittern-mixing pool also can merge, former halogen is through evaporating first precipitated sodium chloride, treat to convert when vitriol is saturated halogen, through evaporation precipitated sodium chloride and epsom salt, when treating that carnallitite is saturated, this bittern is entered evaporative crystallization potassium magnesium mixed salt in the potassium magnesium mixed salt pond.Add the add-on of the saturated solution and a step mother liquor of magnesium chloride when converting halogen, press bittern and form with 15 ℃ of K
+, Na
+, Mg
+ 2∥ Cl
-, So
4 -2H
2The O metastable phase diagram calculates, and the purpose of converting halogen is to regulate bittern to form, and sylvite is not separated out containing the high stage of sodium.And prior art is directly to shine the system kainite through converting halogen under the higher condition of temperature.Because northern China temperature is generally lower, directly solarization system kainite difficulty is bigger, and is inapplicable in China.Convert halogen after evaporation precipitated sodium chloride and epsom salt at bittern-mixing pool, epsom salt is the sal epsom that contains seven crystal water, to being evaporated to carnallitite when saturated, bittern enters and continues evaporation in the potassium magnesium mixed salt pond, separate out a large amount of potassium magnesium mixed salts, the composition of potassium magnesium mixed salt is KCl, KCl, MgCl
2, 6H
2O, MgSo
4, 6H
2O, NaCl.Potassium magnesium mixed salt behind the evaporative crystallization is under the room temperature condition at 10～25 ℃, add fresh water and two step mother liquors to potassium magnesium mixed salt decomposition and inversion, slip gets schoenite and solid potassium chloride after filtering, after the filtration one step mother liquor is put into bittern-mixing pool and is converted halogen usefulness, recyclable vitriolate of tartar and other products wherein.Schoenite and Repone K enter decomposition and inversion two operations, and under 45 °～60 ℃ conditions, adding fresh water is schoenite and Repone K decomposition and inversion the vitriolate of tartar slip, more after filtration, washing, dryly just can get potassium product.In the conventional method, schoenite carries out decomposition and inversion and adds fresh water and also must add Repone K, and among the present invention, decomposition and inversion two does not need to add Repone K and directly adds fresh water and just can obtain potassium product, and its economic benefit is fairly obvious.
Intermediates of the present invention have sodium-chlor; sodium-chlor and epsom salt; three kinds of magnesium chloride saturated bitterns etc.; preceding two kinds is the industrial chemicals of system alkali or other products; a kind of bittern in back is the first-class industrial chemicals of carrying many materials such as boron, lithium, bromine; utilize method of the present invention former halogen can be fully utilized fully, do not have other ejecta basically, not only protected environment effectively but also utilized resource efficiently.This method is not subjected to the temperature condition effect in addition, and it is simple to have operation, and fresh water dosage is few, and energy consumption is little, and production cost is low, does not need flotation agent, does not add Repone K in addition, potassium single rate of recovery height, its mother liquor reusable edible, many advantages such as free from environmental pollution.
Accompanying drawing 1 is a process flow diagram of the present invention.
Embodiment East Platform Ji salt lake brine like this is a vitriolate type bittern, through Exposure to Sunlight elder generation precipitated sodium chloride, when arriving the saturation point of vitriol, bittern is squeezed into bittern-mixing pool for 5.52 tons, convert 4.00 tons bischofite saturated bittern, eliminate the crystallisation stage of schoenite and sylvite, through evaporation anhydrate precipitated sodium chloride and epsom salt, when arriving the saturation point of carnallitite, be that 6.52 tons of saturated halogen of carnallitite enter potassium magnesium mixed salt pond, continue solar evaporation and separate out 1.27 tons the wet ore deposit of potassium magnesium mixed salt the bittern amount.The weight percent in the wet ore deposit of potassium magnesium mixed salt consists of: NaCl8.15%, KCl14.45%, MgCl
219.58%, MgSo
417.93%, B
2O
30.12%, LiCl0.13%, H
2O39.53%.The rate of recovery by former bittern potassium reaches more than 90%.Add 700 kilograms of fresh water 15 ℃ of following decomposition and inversion, slip must wet after filtering 250.18 kilograms in schoenite and Repone K concentrate, the weight percent in this ore deposit consists of: KCl25.90%, K
2So
4, MgSo
46H
2O66.05%, MgCl
2, 6H
2O3.46%, NaCl0.48%, H
2O4.11%.Mix the ore deposit by potassium magnesium, the eduction rate of single potassium is 76.72%.The water that adds 200 kilograms under 55 ℃ carries out decomposition and inversion, washing again after the filtration, dry, 116.58 kilograms potassium product.The product weight percentage composition is: K
2So
497.97%, 97%, KCl0.83%, MgCl
21.13%, NaCl0.04%, other is 0.03% years old.The yield 62.08% of potassium.
Claims (3)
1, a kind of method with preparing potassium sulfate with sulfate type bittern is characterized in that:
(1) technical process is: system potassium magnesium mixed salt → decomposition and inversion one → filtration → decomposition and inversion two → filtration washing → dry packing → potassium product is shone in the salt pan;
(2) processing condition are: the salt pan is shone system potassium magnesium mixed salt operation and is divided into the sodium pond, the system step is shone in three in bittern-mixing pool and potassium magnesium mixed salt pond etc., former halogen evaporation removes and anhydrates and sodium-chlor in the sodium pond, bittern enters bittern-mixing pool when saturated to vitriol, the saturated halogen that adds magnesium chloride in the bittern-mixing pool is regulated the bittern composition, convert halogen ratio=bittern: the saturated halogen of magnesium chloride=1: 0.1～0.8, evaporation removes and anhydrates and sodium-chlor in the bittern-mixing pool, epsom salt, bittern enters potassium magnesium mixed salt pond when saturated to carnallitite, evaporation is anhydrated and is separated out potassium magnesium mixed salt in the potassium magnesium mixed salt pond, when arriving the saturation point of magnesium chloride, carry out solid-liquid separation, Gu Kuang enters down operation; The invert point of decomposition and inversion one operation is 10～25 ℃.45～100% the fresh water that adds wet ore deposit amount is to potassium magnesium mixed salt decomposition and inversion; The temperature inversion of decomposition and inversion two operations is that 45～60 ℃ of fresh water of 55～130% that add wet ore deposits amount are to schoenite and Repone K decomposition and inversion.
2, the method with preparing potassium sulfate with sulfate type bittern according to claim 1 is characterized in that a step mother liquor enters in the bittern-mixing pool, and two step mother liquors are sent into decomposition and inversion one in-process and removed decomposition and inversion potassium magnesium mixed salt.
3, according to claim 1,2 described methods, it is characterized in that sodium pond and bittern-mixing pool merge with preparing potassium sulfate with sulfate type bittern.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95120053A CN1044108C (en) | 1995-11-27 | 1995-11-27 | Method for preparing potassium sulfate with sulfate type bittern |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95120053A CN1044108C (en) | 1995-11-27 | 1995-11-27 | Method for preparing potassium sulfate with sulfate type bittern |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1131639A true CN1131639A (en) | 1996-09-25 |
| CN1044108C CN1044108C (en) | 1999-07-14 |
Family
ID=5082233
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95120053A Expired - Fee Related CN1044108C (en) | 1995-11-27 | 1995-11-27 | Method for preparing potassium sulfate with sulfate type bittern |
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| Country | Link |
|---|---|
| CN (1) | CN1044108C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | Preparation of potassium sulfate from brine containing potassium magnesium sulfate |
| CN1962443B (en) * | 2005-11-10 | 2010-05-12 | 科学与工业研究委员会 | Improved process for the recovery of sulphate of potash (sop) from sulphate rich bittern |
| CN102205978A (en) * | 2011-04-08 | 2011-10-05 | 何茂雄 | Method for producing high-quality sylvine in low cost |
| CN105967211A (en) * | 2016-05-08 | 2016-09-28 | 辽宁工程技术大学 | Method for preparing potassium sulfate from brine |
| CN114735726A (en) * | 2022-02-28 | 2022-07-12 | 广东邦普循环科技有限公司 | Calcium chloride type lithium-containing salt lake brine evaporation and brine mixing mineralization process |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2017281590B2 (en) * | 2016-06-24 | 2019-08-01 | Yara Dallol Bv | Method for the reduction of halite in the preparation of potassium sulphate from potassium-containing ores at high ambient temperatures |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2643001C3 (en) * | 1976-09-24 | 1979-06-07 | Kali Und Salz Ag, 3500 Kassel | Process for the production of potassium sulfate |
| CN1006298B (en) * | 1987-05-26 | 1990-01-03 | 中国科学院青海盐湖研究所 | Method of making schoenite or mixture of schoenite and potassium chloride |
-
1995
- 1995-11-27 CN CN95120053A patent/CN1044108C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | Preparation of potassium sulfate from brine containing potassium magnesium sulfate |
| CN1962443B (en) * | 2005-11-10 | 2010-05-12 | 科学与工业研究委员会 | Improved process for the recovery of sulphate of potash (sop) from sulphate rich bittern |
| CN102205978A (en) * | 2011-04-08 | 2011-10-05 | 何茂雄 | Method for producing high-quality sylvine in low cost |
| CN105967211A (en) * | 2016-05-08 | 2016-09-28 | 辽宁工程技术大学 | Method for preparing potassium sulfate from brine |
| CN105967211B (en) * | 2016-05-08 | 2017-04-19 | 辽宁工程技术大学 | Method for preparing potassium sulfate from brine |
| CN114735726A (en) * | 2022-02-28 | 2022-07-12 | 广东邦普循环科技有限公司 | Calcium chloride type lithium-containing salt lake brine evaporation and brine mixing mineralization process |
| WO2023159899A1 (en) * | 2022-02-28 | 2023-08-31 | 广东邦普循环科技有限公司 | Process for mineralization from evaporation and brine mixing of calcium chloride-type lithium-containing salt lake brine |
| GB2619191A (en) * | 2022-02-28 | 2023-11-29 | Guangdong Brunp Recycling Technology Co Ltd | Process for mineralization from evaporation and brine mixing of calcium chloride-type lithium-containing salt like brine |
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| Publication number | Publication date |
|---|---|
| CN1044108C (en) | 1999-07-14 |
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