CN102249268A - 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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- CN102249268A CN102249268A CN2011101179284A CN201110117928A CN102249268A CN 102249268 A CN102249268 A CN 102249268A CN 2011101179284 A CN2011101179284 A CN 2011101179284A CN 201110117928 A CN201110117928 A CN 201110117928A CN 102249268 A CN102249268 A CN 102249268A
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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 the saturated magnesium chloride bittern of spontaneous evaporation enrichment.
Background technology
Be rich in K, Mg, Na, Cl, SO in the 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 in addition overcast and rainy from air suck-back moisture content also can appear and may; micro-enrichment speed in the bittern can become very slow; being difficult to continue spontaneous evaporation after the materialization attribute of the bittern more complicated that becomes, magnesium chloride reach capacity concentrates.
Summary of the invention
Technical problem to be solved by this invention provides the method for trace element in a kind of saturated magnesium chloride bittern of spontaneous evaporation enrichment that makes micro-enrichment.
For addressing the above problem, the method for trace element in the saturated magnesium chloride bittern of a kind of spontaneous evaporation enrichment of the present invention may further comprise the steps:
(1) spontaneous evaporation is handled: 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 Bittern of Salt Pan is concentrated;
(2) adding KCl handles: after the KCl of purity 〉=98% and distilled water are mixed into pasty state by 1: 0.10～1: 0.11 mass ratio, join in the mashed prod with the speed of 100g/min the old halogen in salt pan described step (1) gained, stir 3～4h, treat to carry out solid-liquid separation after old halogen in salt pan and KCl transform fully, obtain mother liquor and solid phase carnallite; The mass ratio of old halogen in described salt pan and described KCl is 1: 0.10～1: 0.15;
(3) add Na
2SO
4Handle: with the Na of purity 〉=98%
2SO
4After being mixed into pasty state with distilled water by 1: 0.2～1: 0.25 mass ratio, join in the mashed prod, stir 3～4h, treat mother liquor and Na with the speed of 100g/min mother liquor with described step (2) gained
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, make after 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) with the solid phase carnallitite of described step (2), described step (4) and described step (5) gained according to a conventional method through decomposing the Repone K that flotation obtains purity 〉=88.0%.
Principal element mass content in the described step (1) in the old halogen in salt pan of gained is K
+0.04 Mg～0.06%,
2+8.30 Cl～8.60%,
-22.3 SO～22.6%,
4 2-2.80～3.70%, micro-mass ratio is Li 0.0091～0.0098%, B 0.0211～0.0240%.
The principal element mass content is K in the mother liquor of described step (2) gained
+1.50 Mg～2.00%,
2+6.80 Cl～7.10%,
-19.5 SO～20.2%,
4 2-2.80～3.20%, micro-mass ratio is Li0.018～0.021%, B 0.0526～0.0529%.
The principal element mass content is K in the C point mother liquor of the middle gained of described step (3)
+1.85 Mg～1.87%,
2+5.07 Cl～5.10%,
-15.20 SO～15.40%,
4 2-7.00～7.03%, micro-mass ratio is Li 0.010～0.012%, B 0.0269～0.0279%.
The principal element mass content is K in the P point mother liquor of the middle gained of described step (4)
+0.041 Mg～0.200%,
2+7.41 Cl～7.59%,
-19.50 SO～21.0%,
4 2-3.10～3.90%, micro-mass ratio is Li 0.025～0.028%, B 0.0710～0.0714%.
In the 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 Mg～0.10%,
2+7.42 Cl～8.50%,
-19.50 SO～22.50%,
4 2-2.60～3.70%, K
+0.000 Mg～0.050%,
2+7.41 Cl～8.90%,
-19.5 SO～24.0%,
4 2-2.55～3.19%; The trace element mass ratio is followed successively by Li 0.052～0.055%, B 0.1360～0.1367%, Li 0.091～0.094%, B 0.2390～0.2393%.
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
4Handle, therefore, make after magnesium ion in the bittern crystallizes out with other mineral forms, magnesium ion concentration in the liquid phase reduces, thereby make and to proceed spontaneous evaporation under liquid phase part or the situation about stopping very slow and concentrate in bittern spontaneous evaporation speed, micro-lithium in the old halogen, boron etc. constantly obtain enrichment, and the present invention simultaneously has the short advantage of institute's time-consuming than the spontaneous evaporation concentration technology.
2, the present invention not only has after content of magnesium chloride reaches capacity in the bittern, can make trace element reach the characteristics of enrichment, and has the advantages that to continue the enrichment of trace element in the bittern under the situation of atmospheric moisture≤85%.
Embodiment
The method of trace element in the saturated magnesium chloride bittern of embodiment 1 spontaneous evaporation enrichment may further comprise the steps:
(1) spontaneous evaporation is handled: 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 Bittern of Salt Pan is 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 Li 0.0091%, B 0.0211%.
(2) adding KCl handles: get the KCl 2.5Kg of purity 〉=98%, add 0.25kg distilled water and 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, treats to carry out solid-liquid separation after old halogen in salt pan and KCl transform fully, obtains mother liquor 15kg and solid phase carnallitite 7.10kg.
Wherein: the mass ratio of old halogen in salt pan and KCl is 8: 1.
The mass content of principal element is K in the mother liquor
+1.50%, Mg
2+7.10%, Cl
-20.2%, SO
4 2-2.80%, micro-mass ratio is Li 0.018%, B 0.0529%.
(3) add Na
2SO
4Handle: with the Na of purity 〉=98%
2SO
42.8kg, add 0.56kg distilled water and be mixed into pasty state.The mother liquor 15kg that gets in the 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.
The mass content of principal element is K in the C point mother liquor
+1.85%, Mg
2+5.10%, Cl
-15.40%, SO
4 2-7.03%, micro-mass ratio is Li 0.012%, B 0.0279%.
(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 dry out 140 the gram moisture, obtain 5.40kg P point mother liquor, 4.20Kg solid phase (carnallitite, MgSO
47H
2O and NaCl).
Wherein: the principal element mass content is K in the P point mother liquor
+0.041%, Mg
2+7.59%, Cl
-21.0%, SO
4 2-3.90%, micro-mass content is Li 0.028%, B 0.0714%.
(5) P of step (4) gained is selected mother liquor as the old halogen in new salt pan successively set by step (2), step (3), step (4) carry out twice conversion separation, spontaneous evaporation, obtain new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl.
Wherein: the principal element mass content is followed successively by K in the new mother liquor of twice conversion separation, spontaneous evaporation
+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 Li 0.055%, B 0.1360%, Li0.094%, B 0.2393%.
(6) with the solid phase carnallitite of step (2), step (4) and step (5) gained according to a conventional method through decomposing the Repone K that flotation obtains purity 〉=88.0%.
The method of trace element in the saturated magnesium chloride bittern of embodiment 2 spontaneous evaporation enrichments may further comprise the steps:
(1) spontaneous evaporation is handled: 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 Bittern of Salt Pan is 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 Li 0.0098%, B 0.0240%.
(2) adding KCl handles: get the KCl 2.8Kg of purity 〉=98%, add 0.29kg distilled water and 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, treats to carry out solid-liquid separation after old halogen in salt pan and KCl transform fully, obtains mother liquor 16kg and solid phase 6.97kg.
Wherein: the mass ratio of old halogen in salt pan and KCl is 10: 1.
The mass content of the principal element in the mother liquor is K
+2.00%, Mg
2+6.80%, Cl
-19.50%, SO
4 2-3.20%, micro-mass content is Li 0.021%, B 0.0526%.
(3) add Na
2SO
4Handle: the Na that gets purity 〉=98%
2SO
43.0kg, add 0.75kg distilled water and be mixed into pasty state.The mother liquor 20kg that gets in the 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.
The mass content of principal element is K in the C point mother liquor
+1.87%, Mg
2+5.07%, Cl
-15.20%, SO
4 2-7.00%, micro-mass content is Li 0.010%, B 0.0269%.
(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 dry out 170 the gram moisture, obtain the new mother liquor of 6.20kg P point, the 4.30Kg solid phase.
Wherein: the principal element mass content is K in the P point mother liquor
+0.20%, Mg
2+7.41%, Cl
-19.5%, SO
4 2-3.10%, micro-mass content is Li 0.025%, B 0.0710%.
(5) P of step (4) gained is selected mother liquor as the old halogen in new salt pan successively set by step (2), step (3), step (4) carry out twice conversion separation, spontaneous evaporation, obtain new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl.
Wherein: the principal element mass content is followed successively by K in the new mother liquor of twice conversion separation, spontaneous evaporation
+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 Li 0.052%, B 0.1360%, Li0.091%, B 0.2390%.
(6) with the solid phase carnallitite of step (2), step (4) and step (5) gained according to a conventional method through decomposing the Repone K that flotation obtains purity 〉=88.0%.
The method of trace element in the saturated magnesium chloride bittern of embodiment 3 spontaneous evaporation enrichments may further comprise the steps:
(1) spontaneous evaporation is handled: 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 Bittern of Salt Pan is 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 Li 0.0097%, B 0.0232%.
(2) adding KCl handles: get the KCl 2.6Kg of purity 〉=98%, add 0.286kg distilled water and 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, treats to carry out solid-liquid separation after old halogen in salt pan and KCl transform fully, obtains mother liquor 15.6kg and solid phase 6.82kg.
Wherein: the mass ratio of old halogen in salt pan and KCl is 1: 0.15.
The mass content of principal element is K in the mother liquor
+1.85%, Mg
2+7.00%, Cl
-19.90%, SO
4 2-3.00%, micro-mass content is Li 0.020%, B 0.0527%.
(3) add Na
2SO
4Handle: the Na that gets purity 〉=98%
2SO
43.0kg, add 0.66kg distilled water and be mixed into pasty state.The mother liquor 13kg that gets in the 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.
The mass content of principal element is K in the C point mother liquor
+1.86%, Mg
2+5.09%, Cl
-15.3%, SO
4 2-7.02%, micro-mass content is Li 0.011%, B 0.0274%.
(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 dry out 160 the gram moisture, obtain the new mother liquor of 6.00kg P point, the 4.40Kg solid phase.
Wherein: the principal element mass content is K in the P point mother liquor
+0.132%, Mg
2+7.54%, Cl
-20.2%, SO
4 2-3.84%, micro-mass content is Li 0.027%, B 0.0711%.
(5) P of step (4) gained is selected mother liquor as the old halogen in new salt pan successively set by step (2), step (3), step (4) carry out twice conversion separation, spontaneous evaporation, obtain new mother liquor, solid phase carnallitite, MgSO
47H
2O and NaCl.
Wherein: the principal element mass content is followed successively by K in the new mother liquor of twice conversion separation, spontaneous evaporation
+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 Li 0.053%, B 0.1362%, Li 0.093%, B 0.2392%.
(6) with the solid phase carnallitite of step (2), step (4) and step (5) gained according to a conventional method through decomposing the Repone K that flotation obtains purity 〉=88.0%.
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 the bittern after 3 circulations in the foregoing description 1～3 is 〉=and 95%, the enrichment of minor elements Li has reached 51.4%, and the enrichment of B has reached 55.0%.
Claims (6)
1. the method for trace element in the saturated magnesium chloride bittern of spontaneous evaporation enrichment may further comprise the steps:
(1) spontaneous evaporation is handled: 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 Bittern of Salt Pan is concentrated;
(2) adding KCl handles: after the KCl of purity 〉=98% and distilled water are mixed into pasty state by 1: 0.10～1: 0.11 mass ratio, join in the mashed prod with the speed of 100g/min the old halogen in salt pan described step (1) gained, stir 3～4h, treat to carry out solid-liquid separation after old halogen in salt pan and KCl transform fully, obtain mother liquor and solid phase carnallite; The mass ratio of old halogen in described salt pan and described KCl is 1: 0.10～1: 0.15;
(3) add Na
2SO
4Handle: with the Na of purity 〉=98%
2SO
4After being mixed into pasty state with distilled water by 1: 0.2～1: 0.25 mass ratio, join in the mashed prod, stir 3～4h, treat mother liquor and Na with the speed of 100g/min mother liquor with described step (2) gained
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, make after 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) with the solid phase carnallitite of described step (2), described step (4) and described step (5) gained according to a conventional method through decomposing the Repone K that flotation obtains purity 〉=88.0%.
2. the method for trace element in the saturated magnesium chloride bittern of spontaneous evaporation enrichment as claimed in claim 1 is characterized in that: the principal element mass content in the described step (1) in the old halogen in salt pan of gained is K
+0.04 Mg～0.06%,
2+8.30 Cl～8.60%,
-22.3 SO～22.6%,
4 2-2.80～3.70%, micro-mass ratio is Li 0.0091～0.0098%, B 0.0211～0.0240%.
3. the method for trace element in the saturated magnesium chloride bittern of spontaneous evaporation enrichment as claimed in claim 1, it is characterized in that: the principal element mass content is K in the mother liquor of described step (2) gained
+1.50 Mg～2.00%,
2+6.80 Cl～7.10%,
-19.5 SO～20.2%,
4 2-2.80～3.20%, micro-mass ratio is Li 0.018～0.021%, B 0.0526～0.0529%.
4. the method for trace element in the saturated magnesium chloride bittern of spontaneous evaporation enrichment as claimed in claim 1 is characterized in that: the principal element mass content is K in the C point mother liquor of the middle gained of described step (3)
+1.85 Mg～1.87%,
2+5.07 Cl～5.10%,
-15.20 SO～15.40%,
4 2-7.00～7.03%, micro-mass ratio is Li 0.010～0.012%, B 0.0269～0.0279%.
5. the method for trace element in the saturated magnesium chloride bittern of spontaneous evaporation enrichment as claimed in claim 1 is characterized in that: the principal element mass content is K in the P point mother liquor of the middle gained of described step (4)
+0.041 Mg～0.200%,
2+7.41 Cl～7.59%,
-19.50 SO～21.0%,
4 2-3.10～3.90%, micro-mass ratio is Li 0.025～0.028%, B 0.0710～0.0714%.
6. in the saturated magnesium chloride bittern of spontaneous evaporation enrichment as claimed in claim 1 the trace element method, it is characterized in that: in the 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 Mg～0.10%,
2+7.42 Cl～8.50%,
-19.50 SO～22.50%,
4 2-2.60～3.70%, K
+0.000 Mg～0.050%,
2+7.41 Cl～8.90%,
-19.5 SO～24.0%,
4 2-2.55～3.19%; The trace element mass ratio is followed successively by Li 0.052～0.055%, B 0.1360～0.1367%, Li 0.091～0.094%, B 0.2390～0.2393%.
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|---|---|---|---|
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|---|---|---|---|
| CN 201110117928 CN102249268B (en) | 2011-05-04 | 2011-05-04 | Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation |
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| CN102249268A true CN102249268A (en) | 2011-11-23 |
| CN102249268B CN102249268B (en) | 2013-06-05 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106435227A (en) * | 2016-09-09 | 2017-02-22 | 中国科学院青海盐湖研究所 | Method for uranium element enrichment in bittern |
| 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 |
| 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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2011
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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 |
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| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106435227A (en) * | 2016-09-09 | 2017-02-22 | 中国科学院青海盐湖研究所 | Method for uranium element enrichment in bittern |
| 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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| Publication number | Publication date |
|---|---|
| CN102249268B (en) | 2013-06-05 |
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