CN101412524A - Method for separating and extracting potassium chloride from potassium-containing solid mine - Google Patents
Method for separating and extracting potassium chloride from potassium-containing solid mine Download PDFInfo
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- CN101412524A CN101412524A CN 200810232282 CN200810232282A CN101412524A CN 101412524 A CN101412524 A CN 101412524A CN 200810232282 CN200810232282 CN 200810232282 CN 200810232282 A CN200810232282 A CN 200810232282A CN 101412524 A CN101412524 A CN 101412524A
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Abstract
The invention provides a method for separating and extracting potassium chloride by utilizing potassium-containing solid ore. The method comprises the following steps: firstly, potassium-containing sulfurous mixed salt ore obtained by solar evaporation of potassium-containing sulfate saline brine in a brine pan, saturated magnesium chloride brine or unsaturated magnesium chloride brine which is diluted by rainwater, and water are mixed to be prepared into mixed ore, and the mixed ore is stirred and leached at medium and normal temperature and subjected to sodium removal and sulfur removal to obtain a potassium saturated liquid; secondly, the potassium saturated liquid is sent into the brine pan for evaporation until magnesium chloride is saturated, and subjected to liquid-solid separation to obtain low sodium magnesium sulfate and carnallite mixed ore; thirdly, the low sodium magnesium sulfate and the carnallite mixed ore are mixed with the saturated magnesium chloride brine, and subjected to liquid-solid separation to obtain low sodium carnallite; and fourthly, the low sodium carnallite is subjected to water decomposition and solid-liquid separation to obtain the potassium chloride. The product quality indicator (KCl) of the potassium chloride is more than or equal to 90 percent, and the yield of potassium is more than or equal to 60 percent. The method has the advantages that the method has simple technology, cheap and easily-obtained raw materials, low energy consumption and low cost, does not require any floatation agent during the preparation process, is environment-friendly, can treat various low-potassium and high-sulfur minerals, can realize whole year production, and is not limited by climate and meteorologic conditions.
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 the method that raw material is produced Repone K.Mainly be applicable to and adopt the low high sulfur mineral of potassium to produce Repone K.
Background technology
Repone K is the indispensable valuable cargo of industrial and agricultural production.Potassium resource in the salt lake brine is the important source material source of China's sylvite product.The salt lake resources of China is distributed more widely, mainly is distributed in ground such as Qinghai, Xinjiang, Tibet, Sichuan, Inner Mongol, territorial environment condition, resources supplIes and the weather condition that salt lake resources distributes different, and potassium resource required technological method in decision exploitation salt lake is also different.Geographic steam output in salt lake and rainfall amount are the great factors that influences salt lake brine resource separation and Extraction and processing technology.
Summary of the invention
Main purpose of the present invention is for effectively exploitation and the efficiently low steam output of utilization, the geographic salt lake of high rainfall amount potassium resource, and a kind of high rainfall amount area is provided, and (annual rainfall 〉=200mm) salt pan contains the method for the solid ore deposit of potassium separation and Extraction Repone K.
Utilization of the present invention contains the method for the solid ore deposit of potassium separation and Extraction Repone K, be to contain the unsaturated magnesium chloride bittern that potassium sulfate type salt lake bittern salt pan solar evaporation gained contains potassium sulphur mixed salt ore deposit, the firm saturated bittern of magnesium chloride or diluted through rainwater, the water mixing is made into mixed ore deposit, in middle stirring at normal temperature leaching, take off the sodium desulfurization and get the potassium saturated solution; Again the potassium saturated solution is sent into the salt pan and evaporate, the evaporation terminal point is that magnesium chloride is saturated, and liquid-solid separation obtains low sodium sal epsom, carnallitite mixes the ore deposit; To hang down sodium sal epsom, carnallitite then and mix the ore deposit and mix, and mix different substances together and finish the solid and liquid separation and obtain low-sodium carnalite, at last low-sodium carnalite be carried out water decomposition, solid-liquid separation gets Repone K with the magnesium chloride saturated bittern.
The concrete technology of separation and Extraction Repone K of the present invention 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, and the concentration of magnesium chloride bittern is 7.5～8.5%.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.
(2) leaching of the saturated solution of potassium (taking off the sodium desulfurization)
To contain potassium sulfate type salt lake bittern salt pan solar evaporation gained and contain potassium sulphur mixed salt ore deposit, firm saturated bittern of magnesium chloride or the unsaturated magnesium chloride bittern that diluted through rainwater, water is with (1～5): (1～5): the part by weight of (0.1～1) is made into mixed ore deposit, stirs leaching 20～120 minutes at 10～50 ℃; Leaching is finished ore pulp and is carried out solid-liquid separation, and solid phase is the mixture of sodium-chlor and sal epsom, is used to extract sal epsom after the stacking; Liquid phase is the saturated leaching liquid of potassium.
(3) low sodium sal epsom, carnallitite mix producing of ore deposit
The potassium saturated solution is sent into the salt pan evaporate, the evaporation terminal point is that magnesium chloride is saturated, liquid-solid separation, and solid phase is mixed ore deposit (NaCl≤7%) for low sodium sal epsom, carnallitite; Liquid phase chlorination magnesium saturated solution turns back to step (2) recycle.
(4) low-sodium carnalite produces
To hang down sodium sal epsom, carnallitite and mix ore deposit (NaCl≤7%) and magnesium chloride saturated bittern with (1～5): the weight ratio of (5～20) is at 10～50 ℃, stirring was mixed 10～60 minutes, convert and finish slip through solid-liquid separation, solid phase is a low-sodium carnalite, is used for decomposition process and produces Repone K.Mixing different substances together the sodium desulfurization process that takes off that mother liquor turns back to step (2) recycles: firm saturated bittern of magnesium chloride or the unsaturated magnesium chloride bittern that diluted through rainwater, mix different substances together mother liquor, water, contain potassium sulphur mixed salt ore deposit with (1～5): (1～5): (0.1～1): the part by weight of (1～5) is joined the ore deposit.
(5) decomposition of low-sodium carnalite
With low-sodium carnalite and water part by weight with 1:0.1～1, stirred decomposition and inversion 30～90 minutes at 10～30 ℃, decompose and finish slip through solid-liquid separation, solid phase is the Repone K product, and decomposition nut liquid turns back to step (3) and converts halogen: the decomposition nut liquid in the leaching liquid of potassium and low-sodium carnalite ore deposit is with (10～1): the part by weight of (1～10) mixes different substances together.
The Repone K product quality indicator (KCl) 〉=90% of separation and Extraction of the present invention, potassium yield 〉=60%.
The inventive method also can be used for the low-grade carnallite in chloride type salt lake or higher-grade Repone K is produced in the processing of sylvite ore deposit.
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 Repone K;
2, the present invention does not need any flotation agent, environmental protection in producing process;
3, 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 Repone K for the present invention
Embodiment
Further specify the technological process of separation and Extraction Repone K of the present invention below with specific embodiment.
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 contain potassium sulfate type salt lake bittern solar evaporation, separate out sulfur-bearing hydrochlorate carnallite thing (K 〉=5%); Obtain magnesium chloride saturated bittern (concentration of magnesium chloride bittern is 7.5～8.5%) simultaneously.
2. sulfur-bearing hydrochlorate carnallite (K 〉=5%), magnesium chloride saturated bittern, water are pressed (1～5): (1～5): the part by weight of (0.1～2) is made into mixed ore deposit.
3. after above-mentioned mixed ore deposit being stirred 20～90 minutes in 10～50 ℃ of scopes, solid-liquid separation, solid phase are the mixture of sodium-chlor and sal epsom, and liquid phase is the saturated solution of potassium.
4. 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 the low sodium sal epsom of solid phase, the mixed ore deposit of carnallitite; Liquid phase chlorination magnesium saturated solution turns back to 2. recycle of step.
5. will hang down sodium sal epsom, carnallitite and mix ore deposit and the firm saturated bittern of magnesium chloride with (1～5): the part by weight of (5～20) mixes different substances together, and mixes different substances together 10～50 ℃ of temperature, mixes different substances together churning time 10～60 minutes; Mix different substances together and finish the solid and liquid separation, obtain low-sodium carnalite and mix different substances together mother liquor; Low-sodium carnalite removes decomposition process system Repone K, mixes different substances together mother liquor and returns the step sodium desulfurization process that takes off 2. and recycle: unsaturated magnesium chloride bittern, mix different substances together mother liquor, water, contain potassium sulphur mixed salt ore deposit with (1～5): (1～5): (0.1～1): the part by weight of (1～5) is joined the ore deposit.
6. low-sodium carnalite mixes with the part by weight of water with 1:0.1～1, decomposes 30～90 minutes in 10～30 ℃ of scopes, and solid-liquid separation obtains Repone K and decomposition nut liquid; Decomposition nut liquid is got back to the step halogen operation of converting 4. and converted halogen: the decomposition nut liquid in the leaching liquid of potassium and low-sodium carnalite ore deposit is with (10～1): the part by weight of (1～10) mixes different substances together.Mix different substances together and finish liquid and carry out salt pan evaporation, must hang down sodium sal epsom, carnallitite mixes the ore deposit.
Potassium yield 〉=60% that present embodiment is produced, Repone K product quality indicator (KCl) 〉=90%.
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 contain potassium sulfate type salt lake bittern solar evaporation, that separates out sodium chloride-containing, soft potassium magnesium vanadium, sylvite magnesium vanadium, sal epsom, sylvite contains potassium sulfate mineral (K 〉=5%); Obtain magnesium chloride saturated bittern (concentration of magnesium chloride bittern is 7.5～8.5%) simultaneously.
2. will contain potassium sulfate mineral (K 〉=5%), magnesium chloride saturated bittern, water by (1～5): (5～1): the part by weight of (0.1～2) is made into mixed ore deposit.
3. above-mentioned mixed ore deposit was stirred 20～120 minutes in 10～50 ℃ of scopes, solid-liquid separation, solid phase are the mixture of sodium-chlor and sal epsom, and liquid phase is the saturated solution of potassium.
4. the potassium saturated solution is sent into the salt pan evaporation, saturated up to magnesium chloride, solid-liquid separation obtains low sodium sal epsom, carnallitite mixes the ore deposit; Liquid phase chlorination magnesium saturated solution turns back to 2. recycle of step.
5. low sodium sal epsom, carnallitite mix ore deposit and the firm saturated bittern of magnesium chloride with (1～5): the part by weight of (5～20) mixes different substances together, mix different substances together 10～50 ℃ of temperature, mixed different substances together churning time 10～60 minutes, and mixed different substances together and finish the solid and liquid separation, obtain low-sodium carnalite and mix different substances together mother liquor; Low-sodium carnalite removes decomposition process system Repone K, mixing different substances together mother liquor turns back to the step sodium desulfurization process that takes off 2. and recycle: will contain potassium sulfate mineral (K 〉=5%), magnesium chloride saturated bittern, water by (1～5): (5～1): the part by weight of (0.1～2) is made into mixed ore deposit, continues to enter step operation 3. then.
6. low-sodium carnalite and water are with the ratio of 1:0.1～1, in 10～30 ℃ of scopes, decomposed 30～90 minutes, solid-liquid separation, obtain Repone K and decomposition nut liquid, decomposition nut liquid is got back to the step halogen operation of converting 4. and is converted halogen: with potassium saturated solution and decomposition nut liquid with (10～1): the ratio of (1～10) is mixed different substances together, and mixes different substances together to finish liquid and mix different substances together and finish liquid and send into the salt pan evaporation, and is saturated up to magnesium chloride, solid-liquid separation obtains low sodium sal epsom, carnallitite mixes the ore deposit, continues to enter step operation 5..
Potassium yield 〉=60% that present embodiment is produced, Repone K product quality indicator (KCl) 〉=90%.
Claims (3)
1, a kind of utilization contains the method for the solid ore deposit of potassium separation and Extraction Repone K, comprises following processing step:
(1) will contain potassium sulfate type salt lake bittern salt pan solar evaporation gained and contain potassium sulphur mixed salt ore deposit, firm saturated bittern of magnesium chloride or the unsaturated magnesium chloride bittern that diluted through rainwater, water is with (1～5): (1～5): the part by weight of (0.1～1) mixes, stir leaching 20～120 minutes down at 10～50 ℃, solid-liquid separation on ore pulp is finished in leaching, solid phase is the mixture of sodium-chlor and sal epsom, and liquid phase is the saturated leaching liquid of potassium;
(2) the saturated leaching liquid of potassium is sent into the salt pan evaporation, 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 step (3) recycle;
(3) will hang down sodium sal epsom, carnallitite and mix ore deposit and magnesium chloride saturated bittern with (1～5): the weight ratio of (5～20) is mixed, and at 10～50 ℃, stirring was mixed 10～60 minutes, mixes different substances together to finish slip and obtain low-sodium carnalite through solid-liquid separation; Mixing mother liquor returns step (1) and joins the ore deposit;
(4) low-sodium carnalite is mixed with the part by weight of water with 1:0.1～1, stirred decomposition and inversion 30～90 minutes at 10～30 ℃, decompose and finish the slip solid-liquid separation, solid phase is the Repone K product, and decomposition nut liquid turns back to step (2) and converts halogen.
2, utilization contains the method that Repone K is produced in potassium sulphur mixed salt ore deposit according to claim 1, it is characterized in that: in the step (3), the described mother liquor that mixes different substances together returns step (1) circulation and joins the ore deposit, and firm saturated bittern of magnesium chloride or the unsaturated magnesium chloride bittern that diluted through rainwater, mixes different substances together mother liquor, water, contains potassium sulphur mixed salt ore deposit with (1～5): (1～5): (0.1～1): the part by weight of (1～5) is joined the ore deposit.
3, utilization contains the method that Repone K is produced in potassium sulphur mixed salt ore deposit according to claim 1, it is characterized in that: in the step (4), described decomposition nut liquid turns back to step (2) and converts halogen, and the decomposition nut liquid in the leaching liquid of potassium and low-sodium carnalite ore deposit is with (10～1): the weight of (1～10) is mixed, mix different substances together and finish liquid and carry out salt pan evaporation, must hang down sodium sal epsom, carnallitite mixes the ore deposit.
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| CN 200810232282 CN101412524A (en) | 2008-10-30 | 2008-10-30 | Method for separating and extracting potassium chloride from potassium-containing solid mine |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811707A (en) * | 2010-04-16 | 2010-08-25 | 格尔木同兴盐化有限公司 | Method for preparing sodium chloride, potassium chloride, magnesium chloride and magnesium sulfate by utilizing mixed salt mine of salt lake |
| CN102249268A (en) * | 2011-05-04 | 2011-11-23 | 中国科学院青海盐湖研究所 | Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation |
| CN102942196A (en) * | 2012-11-29 | 2013-02-27 | 中国科学院地质与地球物理研究所 | Dressing method fo dense medium in carnallite ore |
| CN103551019A (en) * | 2013-09-25 | 2014-02-05 | 林思源 | Desulphurization technology for utilizing sodium salt in salt making bittern as desulfurizer |
| CN104870669B (en) * | 2012-12-24 | 2018-03-20 | 浦项产业科学研究院 | The method that potassium is extracted from salt solution |
| WO2021223668A1 (en) * | 2020-05-06 | 2021-11-11 | 中国科学院青海盐湖研究所 | Method for using carnallite to prepare potassium chloride |
| CN115215355A (en) * | 2022-08-19 | 2022-10-21 | 中国科学院青海盐湖研究所 | Method for reducing fine sodium chloride in potassium chloride product and application thereof |
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2008
- 2008-10-30 CN CN 200810232282 patent/CN101412524A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811707A (en) * | 2010-04-16 | 2010-08-25 | 格尔木同兴盐化有限公司 | Method for preparing sodium chloride, potassium chloride, magnesium chloride and magnesium sulfate by utilizing mixed salt mine of salt lake |
| CN102249268A (en) * | 2011-05-04 | 2011-11-23 | 中国科学院青海盐湖研究所 | Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation |
| CN102249268B (en) * | 2011-05-04 | 2013-06-05 | 中国科学院青海盐湖研究所 | Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation |
| CN102942196A (en) * | 2012-11-29 | 2013-02-27 | 中国科学院地质与地球物理研究所 | Dressing method fo dense medium in carnallite ore |
| CN102942196B (en) * | 2012-11-29 | 2014-10-15 | 中国科学院地质与地球物理研究所 | Dressing method for dense medium in carnallite ore |
| CN104870669B (en) * | 2012-12-24 | 2018-03-20 | 浦项产业科学研究院 | The method that potassium is extracted from salt solution |
| CN103551019A (en) * | 2013-09-25 | 2014-02-05 | 林思源 | Desulphurization technology for utilizing sodium salt in salt making bittern as desulfurizer |
| CN103551019B (en) * | 2013-09-25 | 2015-11-04 | 林思源 | A kind ofly utilize the sodium salt in the old halogen of salt manufacturing as the sulfur removal technology of desulfurizing agent |
| WO2021223668A1 (en) * | 2020-05-06 | 2021-11-11 | 中国科学院青海盐湖研究所 | Method for using carnallite to prepare potassium chloride |
| US11851340B2 (en) | 2020-05-06 | 2023-12-26 | Qinghai Institute Of Salt Lakes, Chinese Academy Of Sciences | Method for preparing potassium chloride from carnallite |
| CN115215355A (en) * | 2022-08-19 | 2022-10-21 | 中国科学院青海盐湖研究所 | Method for reducing fine sodium chloride in potassium chloride product and application thereof |
| CN115215355B (en) * | 2022-08-19 | 2024-02-23 | 中国科学院青海盐湖研究所 | Method for reducing fine sodium chloride in potassium chloride product and application thereof |
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Open date: 20090422 |