CN102249268B - Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation - Google Patents
Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation Download PDFInfo
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Abstract
The invention relates to a method for enriching trace elements in saturated magnesium chloride brine by natural evaporation. The method comprises the following steps of: (1) naturally evaporating sulfate type salt field brine into old brine in a salt field; (2) adding KCl for treating, and performing solid-liquid separation to obtain a mother liquid and solid-phase carnallite; (3) adding Na2SO4 for treating, and performing solid-liquid separation to obtain a point C mother liquid, solid-phase MgSO4.7H2O and NaCl; (4) naturally evaporating the point C mother liquid to obtain a point P mother liquid, solid-phase carnallite, MgSO4.7H2O and NaCl; (5) performing transformation, separation and natural evaporation on the point P mother liquid twice according to the steps (2), (3) and (4) in sequence to obtain a new mother liquid, solid-phase carnallite, MgSO4.7H2O and NaCl; and (6) performing decomposition and floatation on the solid-phase carnallite obtained in the steps (2), (4) and (5) to obtain potassium chloride. According to the method, the enrichment and concentration of trace elements can be performed continually under the condition that the natural evaporation speed of brine is very low or the natural evaporation stops; meanwhile, the method has the advantage of low time consumption.
Description
Technical field
The present invention relates to the chemical industry of inorganic salt technical field, relate in particular to the method for trace element in spontaneous evaporation enrichment Saturated with Magnesium chloride bittern.
Background technology
Be rich in K, Mg, Na, Cl, SO in sulfate type salt lake bittern
4 2-, and some trace elements, as: lithium, rubidium, bromine, uranium etc.In the old halogen stage; the velocity of evaporation of bittern will become very slowly even in the overcast and rainy possibility that suck-back moisture content from air also can occur; micro-enrichment speed in bittern can become very slow; after reaching capacity, the materialization attribute of the bittern more complicated that becomes, magnesium chloride be difficult to continue spontaneous evaporation concentrated.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for trace element in a kind of spontaneous evaporation enrichment Saturated with Magnesium chloride bittern that makes micro-enrichment.
For addressing the above problem, the method for trace element in a kind of spontaneous evaporation enrichment Saturated with Magnesium chloride bittern of the present invention comprises the following steps:
(1) spontaneous evaporation is processed: the sulfate type Bittern of Salt Pan is through Exposure to Sunlight, spontaneous evaporation, and drying out becomes the old halogen in salt pan after making Bittern of Salt Pan concentrated;
(2) add KCl to process: after the KCl of purity 〉=98% and distilled water are mixed into pasty state by the mass ratio of 1: 0.10～1: 0.11, join in mashed prod with the speed of the 100g/min old halogen in salt pan with described step (1) gained, stir 3～4h, carry out solid-liquid separation after the old halogen in salt pan and KCl transform fully, obtain mother liquor and solid phase carnallite; The mass ratio of the old halogen in described salt pan and described KCl is 1: 0.10～1: 0.15;
(3) add Na
2SO
4Process: with the Na of purity 〉=98%
2SO
4After being mixed into pasty state with distilled water by the mass ratio of 1: 0.2～1: 0.25, join in mashed prod with the speed of the 100g/min mother liquor with described step (2) gained, stir 3～4h, treat mother liquor and Na
2SO
4Carry out solid-liquid separation after transforming fully, obtain C point mother liquor, solid phase MgSO
47H
2O and NaCl; Described mother liquor and described Na
2SO
4Mass ratio be 1: 0.15～1: 0.23;
(4) spontaneous evaporation of C point mother liquor: the C point mother liquor of described step (3) gained is carried out spontaneous evaporation, after making every kilogram of C point mother liquid evaporation moisture 140～170 gram moisture, obtain P point mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl;
(5) the P point mother liquor with described step (4) gained repeats twice conversion separation, spontaneous evaporation by described step (2), step (3), step (4) successively, obtains new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl;
(6) the solid phase carnallitite with described step (2), described step (4) and described step (5) gained obtains the Repone K of purity 〉=88.0% according to a conventional method through decomposing flotation.
Leading ion mass content in described step (1) in the old halogen in salt pan of gained is K
+0.04～0.06%, Mg
2+8.30～8.60%, Cl
-22.3～22.6%, SO
4 2-2.80～3.70%, micro-mass ratio is Li0.0091～0.0098%, B0.0211～0.0240%.
In the mother liquor of described step (2) gained, the leading ion mass content is K
+1.50～2.00%, Mg
2+6.80～7.10%, Cl
-19.5～20.2%, SO
4 2-2.80～3.20%, micro-mass ratio is Li0.018～0.021%, B0.0526～0.0529%.
In the C point mother liquor of the middle gained of described step (3), the leading ion mass content is K
+1.85～1.87%, Mg
2+5.07～5.10%, Cl
-15.20～15.40%, SO
4 2-7.00～7.03%, micro-mass ratio is Li0.010～0.012%, B0.0269～0.0279%.
In the P point mother liquor of the middle gained of described step (4), the leading ion mass content is K
+0.041～0.200%, Mg
2+7.41～7.59%, Cl
-19.50～21.0%, SO
4 2-3.10～3.90%, micro-mass ratio is Li0.025～0.028%, B0.0710～0.0714%.
In described step (5) in the new mother liquor of twice conversion separation, spontaneous evaporation the principal element mass content be followed successively by K
+0.00～0.10%, Mg
2+7.42～8.50%, Cl
-19.50～22.50%, SO
4 2-2.60～3.70%, K
+0.000～0.050%, Mg
2+7.41～8.90%, Cl
-19.5～24.0%, SO
4 2-2.55～3.19%; The trace element mass ratio is followed successively by Li0.052～0.055%, B0.1360～0.1367%, Li0.091～0.094%, B0.2390～0.2393%.
The present invention compared with prior art has the following advantages:
1, because the present invention adds KCl and Na in the old halogen in salt pan
2SO
4Process, therefore, make after magnesium ion in bittern crystallizes out with other mineral forms, magnesium ion concentration in liquid phase reduces, thereby make liquid phase part in the situation that bittern spontaneous evaporation speed is very slow or to stop proceeding spontaneous evaporation concentrated, Trace Element Lithium in old halogen, boron etc. constantly obtain enrichment, and the present invention simultaneously has advantages of that than the spontaneous evaporation concentration technology spent time is short.
2, the present invention not only has after in bittern, content of magnesium chloride reaches capacity, and can make trace element reach the characteristics of enrichment, and have in the situation that atmospheric moisture≤85% can continue bittern in the characteristics of enrichment of trace element.
Embodiment
The method of trace element in embodiment 1 spontaneous evaporation enrichment Saturated with Magnesium chloride bittern comprises the following steps:
(1) spontaneous evaporation is processed: the sulfate type Bittern of Salt Pan is through Exposure to Sunlight, spontaneous evaporation, and drying out becomes the old halogen in salt pan after making Bittern of Salt Pan concentrated.The mass content of the principal element in the old halogen in this salt pan is K
+0.04%, Mg
2+8.30%, Cl
-22.3%, SO
4 2-2.80%, micro-mass ratio is Li0.0091%, B0.0211%.
(2) add KCl to process: to get the KCl2.5Kg of purity 〉=98%, add 0.25kg distilled water to be mixed into pasty state.Get the old halogen 20kg in salt pan, add slowly in mashed prod with the speed of 100g/min, and continue to stir, churning time is 3h, carries out solid-liquid separation after the old halogen in salt pan and KCl transform fully, obtains mother liquor 15kg and solid phase carnallitite 7.10kg.
Wherein: the mass ratio of the old halogen in salt pan and KCl is 8: 1.
In mother liquor, the mass content of leading ion is K
+1.50%, Mg
2+7.10%, Cl
-20.2%, SO
4 2-2.80%, micro-mass ratio is Li0.018%, B0.0529%.
(3) add Na
2SO
4Process: with the Na of purity 〉=98%
2SO
42.8kg, add 0.56kg distilled water to be mixed into pasty state.The mother liquor 15kg that gets in step (2) slowly joins wherein with the speed of 100g/min, and continues to stir, and churning time is 3h, treats mother liquor and Na
2SO
4Carry out solid-liquid separation after transforming fully, obtain 10.7kgC point mother liquor, 7.5kg solid phase (MgSO
47H
2O and NaCl).
Wherein: mother liquor and Na
2SO
4Mass ratio be 75: 14.
In C point mother liquor, the mass content of leading ion is K
+1.85%, Mg
2+5.10%, Cl
-15.40%, SO
4 2-7.03%, micro-mass ratio is Li0.012%, B0.0279%.
(4) spontaneous evaporation of C point mother liquor: the C point mother liquor of step (3) gained is carried out spontaneous evaporation, make every kilogram of C point mother liquid evaporation 140 gram moisture that dry out, obtain 5.40kgP point mother liquor, 4.20Kg solid phase (carnallitite, MgSO
47H
2O and NaCl).
Wherein: in P point mother liquor, the leading ion mass content is K
+0.041%, Mg
2+7.59%, Cl
-21.0%, SO
4 2-3.90%, micro-mass content is Li0.028%, B0.0714%.
(5) P of step (4) gained is selected mother liquor and carry out twice conversion separation, spontaneous evaporation by step (2), step (3), step (4) successively as the old halogen in new salt pan, obtain new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl.
Wherein: in the new mother liquor of twice conversion separation, spontaneous evaporation, the principal element mass content is followed successively by K
+0.00%, Mg
2+8.50%, Cl
-19.5%, SO
4 2-3.70%, K
+0.050%, Mg
2+7.41%, Cl
-19.5%, SO
4 2-2.55%; The trace element mass content is followed successively by Li0.055%, B0.1360%, Li0.094%, B0.2393%.
(6) the solid phase carnallitite with step (2), step (4) and step (5) gained obtains the Repone K of purity 〉=88.0% according to a conventional method through decomposing flotation.
The method of trace element in embodiment 2 spontaneous evaporation enrichment Saturated with Magnesium chloride bitterns comprises the following steps:
(1) spontaneous evaporation is processed: the sulfate type Bittern of Salt Pan is through Exposure to Sunlight, spontaneous evaporation, and drying out becomes the old halogen in salt pan after making Bittern of Salt Pan concentrated.The mass content of the principal element in the old halogen in this salt pan is K
+0.06%, Mg
2+8.60%, Cl
-22.6%, SO
4 2-3.70%, micro-mass content is Li0.0098%, B0.0240%.
(2) add KCl to process: to get the KCl2.8Kg of purity 〉=98%, add 0.29kg distilled water to be mixed into pasty state.Get the old halogen 28kg in salt pan and slowly join wherein with the speed of 100g/min, and continue to stir, churning time is 4h, carries out solid-liquid separation after the old halogen in salt pan and KCl transform fully, obtains mother liquor 16kg and solid phase 6.97kg.
Wherein: the mass ratio of the old halogen in salt pan and KCl is 10: 1.
The mass content of the leading ion in mother liquor is K
+2.00%, Mg
2+6.80%, Cl
-19.50%, SO
4 2-3.20%, micro-mass content is Li0.021%, B0.0526%.
(3) add Na
2SO
4Process: the Na that gets purity 〉=98%
2SO
43.0kg, add 0.75kg distilled water to be mixed into pasty state.The mother liquor 20kg that gets in step (2) slowly joins wherein with the speed of 100g/min, and continues to stir, and churning time is 4h, treats mother liquor and Na
2SO
4Carry out solid-liquid separation after transforming fully, obtain 11.5kg C point mother liquor, 8.1kg solid phase (MgSO
47H
2O and NaCl).
Wherein: mother liquor and Na
2SO
4Mass ratio be 20: 3.
In C point mother liquor, the mass content of leading ion is K
+1.87%, Mg
2+5.07%, Cl
-15.20%, SO
4 2-7.00%, micro-mass content is Li0.010%, B0.0269%.
(4) spontaneous evaporation of C point mother liquor: the C point mother liquor of step (3) gained is carried out spontaneous evaporation, make every kilogram of C point mother liquid evaporation 170 gram moisture that dry out, obtain the new mother liquor of 6.20kg P point, the 4.30Kg solid phase.
Wherein: in P point mother liquor, the leading ion mass content is K
+0.20%, Mg
2+7.41%, Cl
-19.5%, SO
4 2-3.10%, micro-mass content is Li0.025%, B0.0710%.
(5) P of step (4) gained is selected mother liquor and carry out twice conversion separation, spontaneous evaporation by step (2), step (3), step (4) successively as the old halogen in new salt pan, obtain new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl.
Wherein: in the new mother liquor of twice conversion separation, spontaneous evaporation, the principal element mass content is followed successively by K
+0.010%, Mg
2+7.42%, Cl
-22.5%, SO
4 2-2.60%, K
+0.00%, Mg
2+8.90%, Cl
-24.0%, SO
4 2-3.19%; The trace element mass content is followed successively by Li0.052%, B0.1360%, Li0.091%, B0.2390%.
(6) the solid phase carnallitite with step (2), step (4) and step (5) gained obtains the Repone K of purity 〉=88.0% according to a conventional method through decomposing flotation.
The method of trace element in embodiment 3 spontaneous evaporation enrichment Saturated with Magnesium chloride bitterns comprises the following steps:
(1) spontaneous evaporation is processed: the sulfate type Bittern of Salt Pan is through Exposure to Sunlight, spontaneous evaporation, and drying out becomes the old halogen in salt pan after making Bittern of Salt Pan concentrated.The mass content of the principal element in the old halogen in this salt pan is K
+0.05%, Mg
2+8.40%, Cl
-22.5%, SO
4 2-3.22%, micro-mass content is Li0.0097%, B0.0232%.
(2) add KCl to process: to get the KCl2.6Kg of purity 〉=98%, add 0.286kg distilled water to be mixed into pasty state.Get the old halogen 17.3kg in salt pan and slowly join wherein with the speed of 100g/min, and continue to stir, churning time is 3.5h, carries out solid-liquid separation after the old halogen in salt pan and KCl transform fully, obtains mother liquor 15.6kg and solid phase 6.82kg.
Wherein: the mass ratio of the old halogen in salt pan and KCl is 1: 0.15.
In mother liquor, the mass content of leading ion is K
+1.85%, Mg
2+7.00%, Cl
-19.90%, SO
4 2-3.00%, micro-mass content is Li0.020%, B0.0527%.
(3) add Na
2SO
4Process: the Na that gets purity 〉=98%
2SO
43.0kg, add 0.66kg distilled water to be mixed into pasty state.The mother liquor 13kg that gets in step (2) slowly joins wherein with the speed of 100g/min, and continues to stir, and churning time is 4h, treats mother liquor and Na
2SO
4Carry out solid-liquid separation after transforming fully, obtain the 11.5kg mother liquor, 3.9kg solid phase (MgSO
47H
2O and NaCl).
Wherein: mother liquor and Na
2SO
4Mass ratio be 1: 0.23.
In C point mother liquor, the mass content of leading ion is K
+1.86%, Mg
2+5.09%, Cl
-15.3%, SO
4 2-7.02%, micro-mass content is Li0.011%, B0.0274%.
(4) spontaneous evaporation of C point mother liquor: the C point mother liquor of step (3) gained is carried out spontaneous evaporation, make every kilogram of C point mother liquid evaporation 160 gram moisture that dry out, obtain the new mother liquor of 6.00kg P point, the 4.40Kg solid phase.
Wherein: in P point mother liquor, the leading ion mass content is K
+0.132%Mg
2+7.54%, Cl
-20.2%, SO
4 2-3.84%, micro-mass content is Li0.027%, B0.0711%.
(5) P of step (4) gained is selected mother liquor and carry out twice conversion separation, spontaneous evaporation by step (2), step (3), step (4) successively as the old halogen in new salt pan, obtain new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl.
Wherein: in the new mother liquor of twice conversion separation, spontaneous evaporation, the principal element mass content is followed successively by K
+0.00%, Mg
2+8.00%, Cl
-21.5%, SO
4 2-2.64%, K
+0.02%, Mg
2+8.40%, Cl
-23.2%, SO
4 2-3.00%; The trace element mass content is followed successively by Li0.053%, B0.1362%, Li0.093%, B0.2392%.
(6) the solid phase carnallitite with step (2), step (4) and step (5) gained obtains the Repone K of purity 〉=88.0% according to a conventional method through decomposing flotation.
Solid phase and step (5) the gained solid phase purity that has obtained solid phase, step (4) gained of enriching step (2) gained through the trace element in bittern after 3 circulations in above-described embodiment 1～3 is 〉=and 95%, the enrichment that the enrichment of minor elements Li has reached 51.4%, B has reached 55.0%.
Claims (5)
1. the method for trace element in a spontaneous evaporation enrichment Saturated with Magnesium chloride bittern comprises the following steps:
(1) spontaneous evaporation is processed: the sulfate type Bittern of Salt Pan is through Exposure to Sunlight, spontaneous evaporation, and drying out becomes the old halogen in salt pan after making Bittern of Salt Pan concentrated;
(2) add KCl to process: after the KCl of purity 〉=98% and distilled water are mixed into pasty state by the mass ratio of 1: 0.10～1: 0.11, join in mashed prod with the speed of the 100g/min old halogen in salt pan with described step (1) gained, stir 3～4h, carry out solid-liquid separation after the old halogen in salt pan and KCl transform fully, obtain mother liquor and solid phase carnallite; The mass ratio of the old halogen in described salt pan and described KCl is 1: 0.10～1: 0.15;
(3) add Na
2SO
4Process: with the Na of purity 〉=98%
2SO
4After being mixed into pasty state with distilled water by the mass ratio of 1: 0.2～1: 0.25, join in mashed prod with the speed of the 100g/min mother liquor with described step (2) gained, stir 3～4h, treat mother liquor and Na
2SO
4Carry out solid-liquid separation after transforming fully, obtain C point mother liquor, solid phase MgSO
47H2O and NaCl; Described mother liquor and described Na
2SO
4Mass ratio be 1: 0.15～1: 0.23;
(4) spontaneous evaporation of C point mother liquor: the C point mother liquor of described step (3) gained is carried out spontaneous evaporation,
After making every kilogram of C point mother liquid evaporation moisture 140～170 gram moisture, obtain P point mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl;
(5) the P point mother liquor with described step (4) gained repeats twice conversion separation, spontaneous evaporation by described step (2), step (3), step (4) successively, obtains new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl;
(6) the solid phase carnallitite with described step (2), described step (4) and described step (5) gained obtains the Repone K of purity 〉=88.0% according to a conventional method through decomposing flotation.
2. the method for trace element in spontaneous evaporation enrichment Saturated with Magnesium chloride bittern as claimed in claim 1, it is characterized in that: the leading ion mass content in described step (1) in the old halogen in salt pan of gained is K
+0.04～0.06%, Mg
2+8.30～8.60%, Cl
-22.3～22.6%, SO
4 2-2.80～3.70%, micro-mass ratio is Li0.0091～0.0098%, B0.0211～0.0240%.
In spontaneous evaporation enrichment Saturated with Magnesium chloride bittern as claimed in claim 1 the trace element method, it is characterized in that: in the mother liquor of described step (2) gained, the leading ion mass content is K
+1.50～2.00%, Mg
2+6.80～7.10%, Cl
-19.5～20.2%, SO
4 2-2.80～3.20%, micro-mass ratio is Li0.018～0.021%, B0.0526～0.0529%.
4. the method for trace element in spontaneous evaporation enrichment Saturated with Magnesium chloride bittern as claimed in claim 1 is characterized in that: in described step (3) in the C point mother liquor of gained the leading ion mass content be K
+1.85～1.87%, Mg
2+5.07～5.10%, Cl
-15.20～15.40%, SO
4 2-7.00～7.03%, micro-mass ratio is Li0.010～0.012%, B0.0269～0.0279%.
5. the method for trace element in spontaneous evaporation enrichment Saturated with Magnesium chloride bittern as claimed in claim 1 is characterized in that: in described step (4) in the P point mother liquor of gained the leading ion mass content be K
+0.041～0.200%, Mg
2+7.41～7.59%, Cl
-19.50～21.0%, SO
4 2-3.10～3.90%, micro-mass ratio is Li0.025～0.028%, B0.0710～0.0714%.
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| CN105399456A (en) * | 2015-12-25 | 2016-03-16 | 茫崖兴元钾肥有限责任公司 | Novel technology for preparing potash magnesium sulphate fertilizer by reaction between magnesium sulfate ore and potassium chloride |
| CN106435227B (en) * | 2016-09-09 | 2018-10-02 | 中国科学院青海盐湖研究所 | The enrichment method of uranium element in a kind of brine |
| CN110713195A (en) * | 2019-11-27 | 2020-01-21 | 青海民族大学 | Method for improving production efficiency of chloride type salt pan and chloride type salt pan product |
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| CN1335260A (en) * | 2001-09-07 | 2002-02-13 | 中信国安锂业科技有限责任公司 | Halogenation process of preparing KCl |
| CN1439602A (en) * | 2002-09-25 | 2003-09-03 | 新疆罗布泊钾盐科技开发有限责任公司 | Preparation of potassium sulfate from brine containing potassium magnesium sulfate |
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| CN101412524A (en) * | 2008-10-30 | 2009-04-22 | 中国科学院青海盐湖研究所 | Method for separating and extracting potassium chloride from potassium-containing solid mine |
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| CN1335260A (en) * | 2001-09-07 | 2002-02-13 | 中信国安锂业科技有限责任公司 | Halogenation process of preparing KCl |
| CN1439602A (en) * | 2002-09-25 | 2003-09-03 | 新疆罗布泊钾盐科技开发有限责任公司 | Preparation of potassium sulfate from brine containing potassium magnesium sulfate |
| CN1724370A (en) * | 2005-07-17 | 2006-01-25 | 青海中信国安科技发展有限公司 | Process for producing potassium chloride by sulfate type potassium-containing halogen water |
| CN101412524A (en) * | 2008-10-30 | 2009-04-22 | 中国科学院青海盐湖研究所 | Method for separating and extracting potassium chloride from potassium-containing solid mine |
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