CN101412639A - Method for preparing potash magnesium sulphate fertilizer from potassium-containing solid mine by separation and extraction - Google Patents
Method for preparing potash magnesium sulphate fertilizer from potassium-containing solid mine by separation and extraction Download PDFInfo
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- CN101412639A CN101412639A CN 200810232285 CN200810232285A CN101412639A CN 101412639 A CN101412639 A CN 101412639A CN 200810232285 CN200810232285 CN 200810232285 CN 200810232285 A CN200810232285 A CN 200810232285A CN 101412639 A CN101412639 A CN 101412639A
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Abstract
The invention provides a method for utilizing potassic solid ore to separate and extract potash magnesium sulphate fertilizer. The method comprises the following steps: potassic sulphate ore and magnesium chloride saturated brine which are obtained through solarizing and evaporating a brine saltern in a potassic sulphate type saline are used as raw materials; potassium in the potassic sulphate ore is salted out and leached through the magnesium chloride saturated brine to obtain a saturated potassium solution; the saturated potassium solution is added with the brine saltern and is evaporated to prepare low-sodium magnesium sulfate and carnallite mixed ore; and the low-sodium magnesium sulfate and the carnallite mixed ore are decomposed and transformed to obtain the potash magnesium sulphate fertilizer. The potash magnesium sulphate fertilizer prepared through the method meets the national GB/T20937-2002 standard for a qualified product; and the yield of potassium is more than or equal to 60 percent. The method is suitable for processing the potassic sulphate type saline brine or the chloride type brine saltern ore with low yield of carnallite prepared through the addition of halogen, as the concentration of the potassic saturated brine potassium obtained through evaporating the brine saltern of the potassic sulphate type saline can not be ensured by the influence of rainfall amount, and magnesium chloride is unsaturated or has unhigh concentration due to that ,the magnesium chloride saturated brine is influenced by the factor of rainfall .
Description
Technical field
The invention belongs to the salt chemical engineering technical field, relate to a kind of inorganic salt phase chemistry isolation technique, be specifically related to a kind ofly contain potassium bittern solar evaporation gained with the magnesium sulfate salt lake and contain that potassium sulfuric acid salt mine mixes the ore deposit, just saturated or lower concentration chlorination magnesium bittern is raw material, by the leaching of saltouing, filtering separation, decomposition and inversion are produced the method for potash magnesium sulphate fertilizer.
Background technology
The chemical molecular formula of potash magnesium sulphate fertilizer: K
2SO
4MgSO
46H
2O is the inorganic green fertilizer of a kind of K of being rich in, Mg, three kinds of nutrients of S, and the ratio between the three is very stable, and its important character is solubility good (100% is water-soluble), when soil nutrient deficiency, can provide part potassium and whole sulphur, magnesium nutrient; Another important character of potash magnesium sulphate fertilizer is to be chemically neutral salt, and not using to influence soil pH value.Owing to consist of sulfate radical, chloride content is low, thereby its salt index is relatively low, and life-time service is less to the influence of soil salinity.Potash magnesium sulphate fertilizer is specially adapted to the fertilising of fear-chlorion crop, can increase the yield and quality of economic farm crop.
China's sulfate type salt lake potassium resource total reserves accounts for 40～60% of national salt lake potassium resource total reserves, and sulfate type salt lake contains potassium bittern resulting mixing salt mineralogical composition complexity in the solar evaporation process of salt pan.By the end of the late 20th century, the technology that contains separation and Extraction potash magnesium sulphate fertilizer the potassium vitriol mixing saline minerals from salt pan evaporation gained does not have important breakthrough always.The late 20th century, initial stage 21st century; because agriculture production is to the active demand of potash fertilizer; the technical field of domestic related scientific research department separation and Extraction potash magnesium sulphate fertilizer in containing potassium vitriol mixing saline minerals has had important breakthrough; emerged a lot of methods, certain methods has been used for large-scale production.
China salt lake is numerous, and the residing climatope in salt lake is complicated and changeable.Geographic steam output in salt lake and rainfall amount greatly affect the selection of salt lake brine resource separation and Extraction and processing technology and use.
Summary of the invention
Main purpose of the present invention provides a kind of utilization and contains potassium sulfuric acid salt mine (or solubility contains sylvite ore) magnesium chloride bittern stirring leaching potassium, the potassium leaching liquid is converted the evaporation of halogen field and is obtained low sodium sal epsom, the mixed ore deposit of carnallitite, and low sodium sal epsom, carnallitite mix the method that the ore deposit decomposition and inversion is produced potash magnesium sulphate fertilizer.
The present invention obtains the potassium saturated solution by the magnesium chloride bittern potassium that contains in the potassium sulfuric acid salt mine of leaching of saltouing; The potassium saturated solution is converted the evaporation of halogen field and is made low sodium sal epsom, the mixed ore deposit of carnallitite; Low sodium sal epsom, carnallitite mix the ore deposit decomposition and inversion and obtain potash magnesium sulphate fertilizer, and its concrete preparation technology is as follows:
1. feedstock production: it is saturated to potassium up to bittern to contain potassium sulfate type salt lake bittern salt pan solar evaporation, solid-liquid separation; Separate back potassium saturated bittern revaporization to saturated to magnesium chloride, solid-liquid separation obtains raw material Gu Kuang (containing potassium sulphur mixed salt ore deposit) and the firm saturated bittern of magnesium chloride respectively.The essential mineral that gained contains potassium sulphur mixed salt ore deposit constitutes: sodium-chlor, sal epsom, soft potassium magnesium vanadium, sylvite magnesium vanadium, sylvite etc., or for there not being other potassium-bearing mineral mixture of sylvite ore deposit or sylvite magnesium vanadium; Or for being other type soluble potassium potassium-bearing mineral.The concentration of magnesium chloride bittern is 7.5～8.5%.
2. the leaching of potassium saturated solution: unsaturated magnesium chloride bittern, the water that dilute with the firm saturated bittern of magnesium chloride or through rainwater, contain potassium sulphur mixed salt ore deposit with (1～5): (0.1～1): the part by weight mixing of (1～5), stirred 20～90 minutes at 10～50 ℃, leaching contains the potassium in the potassium sulphur mixed salt ore deposit, solid-liquid separation on ore pulp is finished in leaching, and solid phase is the mixture of sodium-chlor and sal epsom; Liquid phase is the saturated leaching liquid of potassium.
3. low sodium sal epsom, carnallitite mix producing of ore deposit: the saturated leaching liquid of potassium is sent into the salt pan evaporation, and the evaporation terminal point is that magnesium chloride is saturated, liquid-solid separation, and solid phase is mixed the ore deposit for low sodium sal epsom, carnallitite; Liquid phase chlorination magnesium saturated solution turns back to 2. recycle of step.
4. low sodium sal epsom, carnallitite mix the decomposition and inversion in ore deposit: low sodium sal epsom, the mixed ore deposit of carnallitite and water carry out one section decomposition and inversion with the part by weight of 1:0.1～1:1, obtain one section and transform solid phase; One section transforms solid phase and carries out two sections decomposition and inversion with water with the part by weight of 1:0.1～1:2 again, and two sections conversions are finished the slip solid-liquid separation and obtained potash magnesium sulphate fertilizer; Wherein one section, two sections decomposition and inversion temperature are 10～50 ℃, and the decomposition and inversion time is 10～90 minutes.
One section, two sections transform mother liquor turn back to step 3. with the halogen of converting of potassium saturated solution, mix different substances together ratio (weight ratio) and be: one section decomposed solution: two sections decomposed solution: potassium saturated solution=(1～5): (1～5): (5～1).Mix different substances together and finish liquid and carry out the salt pan and evaporate to such an extent that low sodium sal epsom, carnallitite mix the ore deposit.
The potash magnesium sulphate fertilizer of the present invention's preparation, quality product meets national GB/T20937-2002 salable product standard, potassium yield 〉=60%.
The inventive method is suitable for containing potassium sulfate type salt lake bittern salt pan evaporation gained and contains potassium saturated bittern potassium concn and can not get assurance because of influenced by rainfall amount, gained magnesium chloride saturated bittern concentration because of be subjected to rainfall factor affecting magnesium chloride and be in unsaturated or concentration not high, convert stew in soy sauce and be equipped with the lower processing that contains potassium sulfate type salt lake bittern or ore deposit, chloride type bittern salt pan of carnallitite yield.
The present invention compared with prior art has the following advantages:
1, technology of the present invention is simple, and raw material is cheap and easy to get, and energy consumption is lower, and cost is lower, the yield height of separation and Extraction potash magnesium sulphate fertilizer;
2, two sections decomposition and inversion mother liquid recyclings of the present invention improve the potassium yield, have effectively saved salt lake resources;
3, the present invention does not need any flotation agent, environmental protection in producing process;
4, Technological adaptability of the present invention is strong, can handle the high sulfur mineral of various low potassium, can realize the production of the property whole year, not limited by weather, meteorological conditions.
Description of drawings
Fig. 1 produces the process flow sheet of potash magnesium sulphate fertilizer for the present invention
Embodiment
With embodiment technological process of the present invention is described below:
Embodiment 1
1. be that gold is helped Na with the chemical constitution system point, K, Mg ∥ Cl, SO4-H2O15 ℃ or 25 ℃ metastable phase diagram sal epsom phase region to contain potassium sulfate type salt lake bittern solar evaporation saturated to potassium up to bittern, solid-liquid separation; Separate back potassium saturated bittern revaporization to saturated to magnesium chloride, solid-liquid separation obtains raw material Gu Kuang (containing potassium sulphur mixed salt ore deposit) and the firm saturated bittern of magnesium chloride respectively.Gained contains K 〉=5% in potassium sulphur mixed salt ore deposit; The concentration of magnesium chloride bittern is 7.5～8.5%.
2. sulfur-bearing hydrochlorate carnallite (K 〉=5%), the firm saturated bittern of magnesium chloride (getting bittern through being in undersaturated condition after the rainwater dilution), water are pressed (1～5): (5～1): the part by weight of (0.1～2) is made into mixed ore deposit; To mix the ore deposit and stir leaching 20～90 minutes at 10～50 ℃, solid-liquid separation, solid phase are the mixture of sodium-chlor and sal epsom, and liquid phase is the saturated solution of potassium.
3. the potassium saturated solution is sent into the salt pan and evaporate, it is saturated to be evaporated to magnesium chloride, and the slip solid-liquid separation is finished in evaporation, obtains low sodium sal epsom, the mixed ore deposit of carnallitite; The magnesium chloride saturated bittern returns step and 2. circulates.
4. will hang down sodium sal epsom, the mixed ore deposit of carnallitite and water and at first carry out first section decomposition and inversion: the mineral water ratio of first section decomposition and inversion is: 1:.1～1:1,10～90 minutes decomposition and inversion time, 10～50 ℃ of decomposition and inversion temperature; The slip solid-liquid separation is finished in first section conversion, obtain one section and transform solid phase, one section transforms solid phase and carries out second section decomposition and inversion with water: the mineral water of second section decomposition and inversion is than being 1:0.1～1:2, and the decomposition and inversion time is 10～90 minutes, 10～50 ℃ of decomposition and inversion temperature; Two sections conversions are finished the slip solid-liquid separation and are obtained potash magnesium sulphate fertilizer;
One section, two sections transform mother liquor turn back to step 4. with the halogen of converting of potassium saturated solution, mix different substances together ratio (weight ratio) and be: one section decomposed solution: two sections decomposed solution: potassium saturated solution=(1～5): (1～5): (5～1).Mix different substances together and finish liquid and carry out the salt pan and evaporate to such an extent that low sodium sal epsom, carnallitite mix the ore deposit.
Quality product meets national GB/T20937-2002 salable product standard, potassium yield 〉=60%.
Embodiment 2
1. the chemical constitution system point is that gold is helped Na, K, Mg ∥ Cl, SO4-H2O15 ℃ or the 25 ℃ soft potassium magnesium of metastable phase diagram vanadium phase region to contain potassium sulfate type salt lake bittern solar evaporation saturated to potassium up to bittern, solid-liquid separation; Separate back potassium saturated bittern revaporization to saturated to magnesium chloride, solid-liquid separation obtains raw material Gu Kuang (containing potassium sulphur mixed salt ore deposit) and the firm saturated bittern of magnesium chloride respectively.Gained contains K 〉=5% in potassium sulphur mixed salt ore deposit; The concentration of magnesium chloride bittern is 7.5～8.5%.
2. gained is contained potassium sulfate mineral, magnesium chloride saturated bittern (or get bittern through being in undersaturated condition after the rainwater dilution), water by (1～5): (5～1): the part by weight of (0.1～2) is made into mixed ore deposit, to mix the ore deposit again stirred 20～120 minutes in 10～50 ℃ of scopes, solid-liquid separation, solid phase is the mixture of sodium-chlor and sal epsom, and liquid phase is the saturated solution of potassium.
3. the potassium saturated solution is sent into the salt pan and evaporate, it is saturated to be evaporated to magnesium chloride, and the slip solid-liquid separation is finished in evaporation, obtains low sodium sal epsom, the mixed ore deposit of carnallitite; The magnesium chloride saturated bittern returns step and 2. circulates.
4. will hang down sodium sal epsom, the mixed ore deposit of carnallitite and water and at first carry out first section decomposition and inversion: the mineral water of first section decomposition and inversion is than being 1:0.1～1:1,10～90 minutes decomposition and inversion time, 10～50 ℃ of decomposition and inversion temperature; The slip solid-liquid separation is finished in first section conversion, obtains one section and transforms solid phase; One section transforms solid phase and carries out second section decomposition and inversion with water: the mineral water of second section decomposition and inversion is than being 1:0.1～1:2,10～90 minutes decomposition and inversion time, 10～50 ℃ of decomposition and inversion temperature; Two sections conversions are finished the slip solid-liquid separation and are obtained potash magnesium sulphate fertilizer.
One section, two sections transform mother liquor turn back to step 4. with the halogen of converting of potassium saturated solution, mix different substances together ratio (weight ratio) and be: one section decomposed solution: two sections decomposed solution: potassium saturated solution=(1～5): (1～5): (5～1).Mix different substances together and finish liquid and carry out the salt pan and evaporate to such an extent that low sodium sal epsom, carnallitite mix the ore deposit.
Quality product meets national GB/T20937-2002 salable product standard, potassium yield 〉=60%.
Claims (3)
1, a kind of utilization contains the method for the solid ore deposit of potassium separation and Extraction potash magnesium sulphate fertilizer, is to be finished by following processing step:
1. it is saturated to potassium up to bittern to contain potassium sulfate type salt lake bittern salt pan solar evaporation, solid-liquid separation; Separate back potassium saturated bittern revaporization to saturated to magnesium chloride, solid-liquid separation obtains containing potassium sulphur mixed salt Gu Kuang and the firm saturated bittern of magnesium chloride respectively;
2. unsaturated magnesium chloride bittern, the water that dilute with the firm saturated bittern of magnesium chloride or through rainwater, contain potassium sulphur mixed salt Gu Kuang with (1～5): (0.1～1): the part by weight mixing of (1～5), stirred 20～90 minutes at 10～50 ℃, leaching contains the potassium in the potassium sulphur mixed salt ore deposit, solid-liquid separation on ore pulp is finished in leaching, and solid phase is the mixture of sodium-chlor and sal epsom; Liquid phase is the saturated leaching liquid of potassium;
3. the saturated leaching liquid of potassium is sent into the salt pan evaporation, and the evaporation terminal point is that magnesium chloride is saturated, liquid-solid separation, and solid phase is mixed the ore deposit for low sodium sal epsom, carnallitite; Liquid phase chlorination magnesium saturated solution turns back to 2. recycle of step;
4. low sodium sal epsom, the mixed ore deposit of carnallitite and water carry out one section decomposition and inversion with the part by weight of 1:0.1～1:1, obtain one section and transform solid phase; One section transforms solid phase and carries out two sections decomposition and inversion with water with the part by weight of 1:0.1～1:2 again, and two sections conversions are finished the slip solid-liquid separation and obtained potash magnesium sulphate fertilizer; One section, two sections conversion mother liquors turn back to step and 3. convert halogen with the potassium saturated solution.
2, utilize the method that contains the solid ore deposit of potassium separation and Extraction potash magnesium sulphate fertilizer according to claim 1, it is characterized in that: 4. described one section, two sections decomposition and inversion temperature of step are 10～50 ℃, and the decomposition and inversion time is 10～90 minutes.
3, utilize the method that contains the solid ore deposit of potassium separation and Extraction potash magnesium sulphate fertilizer according to claim 1, it is characterized in that: 4. described one section, two sections decomposed solution of step and step potassium saturated solution 3. are with (1～5): (1～5): the part by weight of (5～1) mixes different substances together, and mixes different substances together to finish liquid and carry out the salt pan and evaporate to such an extent that low sodium sal epsom, carnallitite mix the ore deposit.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102322856A CN101412639B (en) | 2008-10-30 | 2008-10-30 | Method for preparing potash magnesium sulphate fertilizer from potassium-containing solid mine by separation and extraction |
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| CN2008102322856A CN101412639B (en) | 2008-10-30 | 2008-10-30 | Method for preparing potash magnesium sulphate fertilizer from potassium-containing solid mine by separation and extraction |
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| CN101412639B CN101412639B (en) | 2011-06-22 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350399A (en) * | 2011-07-04 | 2012-02-15 | 中蓝连海设计研究院 | Desliming method for low-grade earth surface solid potassium ores |
| CN102826874A (en) * | 2012-09-04 | 2012-12-19 | 青海中信国安科技发展有限公司 | Method for producing potash magnesium sulphate fertilizers with unsaturation brine serving as flotation medium |
| CN107381603A (en) * | 2017-07-28 | 2017-11-24 | 中国科学院青海盐湖研究所 | The preparation method of picromerite based on adding halogen method |
| CN107935637A (en) * | 2017-11-10 | 2018-04-20 | 国投新疆罗布泊钾盐有限责任公司 | A kind of method for producing top grade potassic-magnesian fertilizer |
| CN111362731A (en) * | 2020-05-06 | 2020-07-03 | 中国科学院青海盐湖研究所 | Potassium magnesium sulfate fertilizer, potassium chloride and preparation method of potassium sulfate |
| CN113135581A (en) * | 2021-06-01 | 2021-07-20 | 吉林海资生物工程技术有限公司 | Process for preparing magnesium potassium sulfate and potassium sulfate by extracting potassium from corn soaking liquid |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3589871A (en) * | 1968-06-10 | 1971-06-29 | Great Salt Lake Minerals | Method for the production of high-grade kainite |
| CN1195710C (en) * | 2003-08-29 | 2005-04-06 | 青海中信国安科技发展有限公司 | Method of producing potassium sulfate magnesium fertilizer |
| 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 |
| CN101157460B (en) * | 2007-08-28 | 2010-09-01 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride by employing sulfate type salt lake potassium-containing brine |
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2008
- 2008-10-30 CN CN2008102322856A patent/CN101412639B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350399A (en) * | 2011-07-04 | 2012-02-15 | 中蓝连海设计研究院 | Desliming method for low-grade earth surface solid potassium ores |
| CN102350399B (en) * | 2011-07-04 | 2013-09-04 | 中蓝连海设计研究院 | Desliming method for low-grade earth surface solid potassium ores |
| CN102826874A (en) * | 2012-09-04 | 2012-12-19 | 青海中信国安科技发展有限公司 | Method for producing potash magnesium sulphate fertilizers with unsaturation brine serving as flotation medium |
| CN102826874B (en) * | 2012-09-04 | 2014-01-01 | 青海中信国安科技发展有限公司 | Method for producing potash magnesium sulphate fertilizers with unsaturation brine serving as flotation medium |
| CN107381603A (en) * | 2017-07-28 | 2017-11-24 | 中国科学院青海盐湖研究所 | The preparation method of picromerite based on adding halogen method |
| CN107935637A (en) * | 2017-11-10 | 2018-04-20 | 国投新疆罗布泊钾盐有限责任公司 | A kind of method for producing top grade potassic-magnesian fertilizer |
| CN111362731A (en) * | 2020-05-06 | 2020-07-03 | 中国科学院青海盐湖研究所 | Potassium magnesium sulfate fertilizer, potassium chloride and preparation method of potassium sulfate |
| CN111362731B (en) * | 2020-05-06 | 2021-11-02 | 中国科学院青海盐湖研究所 | Potassium magnesium sulfate fertilizer, potassium chloride and preparation method of potassium sulfate |
| CN113135581A (en) * | 2021-06-01 | 2021-07-20 | 吉林海资生物工程技术有限公司 | Process for preparing magnesium potassium sulfate and potassium sulfate by extracting potassium from corn soaking liquid |
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| CN101412639B (en) | 2011-06-22 |
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