CN1304293C - Preparation of potassium chloride by multi-component crystallization of solid mineral production by dissolving and leaching process - Google Patents
Preparation of potassium chloride by multi-component crystallization of solid mineral production by dissolving and leaching process Download PDFInfo
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- CN1304293C CN1304293C CNB021339163A CN02133916A CN1304293C CN 1304293 C CN1304293 C CN 1304293C CN B021339163 A CNB021339163 A CN B021339163A CN 02133916 A CN02133916 A CN 02133916A CN 1304293 C CN1304293 C CN 1304293C
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- crystallization
- halogen
- dissolving
- leaching
- potassium
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Abstract
The present invention provides a preparation method of potassium chloride by multi-component crystallization of solid mineral production by dissolving and leaching processes. Waste liquid, waste salt and waste water generated in the process of processing carnallite are used as dissolving and leaching liquid for carrying out selective dissolving and leaching mining in order to simultaneously mine halogen liquid abundant with potassium chloride from solid sylvite ore when sodium chloride and magnesium chloride are not mined; the potassium chloride with high quality can be directly obtained by one-step through a crystallization technology. Simultaneously, the dissolving and leaching liquid prepared by the waste liquid in a crystallization process is injected back in ore bodies for circulating mining. The waste water is used circularly and any waste water and waste material are not discharged. Therefore, the present invention does not pollute the environment or damage the ground and the vegetation, and can effectively reduce production cost. The characteristics and the advantages of various crystallization technologies are sufficiently exerted through the organic and skillful combination of multi-component crystallization technologies; simultaneously, the valent potassium chloride can be repeatedly recovered for obtaining potassium chloride products which are convenient for deep processing and have high quality and coarse granularity for effectively enhancing product yield and reducing energy consumption.
Description
Technical field
The present invention relates to a kind of from solid sylvite mineral the method for direct production Repone K, belong to solid mineral solution mining and processing technique field.
Background technology
At present, the exploitation to the solid sylvite ore both at home and abroad has the underground mining of comprising and opencast solid phase extraction system, and the liquid phase exploitation then comprises CL and two kinds of extraction systems of selective dissolution.Though solid phase exploitation throughput is big, the work efficiency height, the back production cost is low, main equipment operation easy to use, but initial cost and ore extraction amount are big, and the ore loss ratio and the rate of dilution are higher, and the face of land and vegetation deterioration thereof are serious, and in recovery process, impure mineral is also come out by exploitation with valuable mineral, not only environment is polluted and destroys, and increase postorder amount of finish and difficulty of processing, therefore, be not suitable for exploiting low-grade sylvite ore.Though liquid phase exploitation initial cost is little, cost of winning is low, valuable mineral rate of recovery height, the barren rock quantum of output is few, exploit safe, environmental pollution is little, floor space is little, and is little to the face of land and vegetation deterioration thereof, but because the exploitation of existing liquid phase uses fresh water as solvent mostly, in extraction Repone K, still want a large amount of magnesium chloride of extraction and sodium-chlor, this is concerning the Laos's carnallite that is rich in magnesium chloride, and it is big not only to exploit difficulty, and economic benefit is low, is a difficult problem to the tighter Mekong River valley of environmental requirement especially.
Summary of the invention
The object of the present invention is to provide a kind of investment little, cost is low, and rate of recovery height is free from environmental pollution, does not destroy selectivity production by dissolving and leaching process-multi-component crystallization method of the face of land and vegetation thereof.
The present invention utilizes the waste liquid that produces in the carnallitite course of processing, abraum salt, waste water as leaching solution, carry out the selectivity production by dissolving and leaching process, so that in not extraction sodium-chlor and magnesium chloride, only the saltwater brine of Repone K is rich in extraction from solid sylvite ore, and directly obtains high-quality Repone K by one step of crystallization processes.
The present invention realizes by following process steps: it comprises the selectivity production by dissolving and leaching process, and with the potassium-rich brine evaporative crystallization that exploitation is come out, it is characterized in that:
The used leaching solution of selectivity production by dissolving and leaching process is made up of the chemical composition of following weight percent:
Repone K≤0.4%
Sodium-chlor 1.8-2%
Magnesium chloride 24.5-26%
Surplus is abraum salt liquid and water;
Leaching solution temperature: 25-60 ℃;
Molten compregnate power: 1 meter of the every decline of hole depth, required surface pressure is 0.115kg/cm
2
Leaching solution goes out halogen amount: 200-450m
3/ hour;
The rich potassium saltwater brine that exploitation is come out is directly through following crystallization processes step:
1, under 30-145 ℃ of temperature condition, carry out evaporative crystallization, vaporize water returns the leaching solution pond; Crystallization precipitate through separate sodium chloride-containing high temp. salt and analyse the salt mother liquor, high temp. salt returns molten soaking pit;
2, under 20-40 ℃ of temperature condition, the above-mentioned salt mother liquor of analysing is carried out crystallisation by cooling, separate out low-sodium carnalite, isolate low-sodium carnalite after, obtaining main component is the old halogen of magnesium chloride;
3, under 15-40 ℃ of temperature condition, feed intake by following weight ratio: carnallitite: water: convert halogen carnallitite=1: 0.5: 4-6, control fast decomposition and crystallization, control stirring velocity 50-100rpm, 60-90 minute crystallization reaction time, isolate thick potassium after, decomposition nut liquid;
4, the old halogen of 2 steps and the decomposition nut liquid of 3 steps are converted the halogen crystallization, control stirring velocity 100-300rpm reaction times 30-70 minute, converts halogen and compares M
25: F=1: 2, crystallization gets carnallitite slip and convert the halogen mother liquor, converts the halogen mother liquor and returns molten soaking pit, and the carnallitite slip returns 3 steps again to be controlled fast decomposition and crystallization and goes out thick potassium;
5, will return molten soaking pit vaporize water, high temp. salt, convert the halogen mother liquor and be mixed with to be recycled into behind the leaching solution and carry out the selectivity exploitation in the ore body.
Described leaching solution flow velocity and flow will be according to moltenly soaking time, temperature, adopting index such as halogen amount and determine; Described leaching solution goes out the halogen amount and then determines according to industrial scale; The described molten time of soaking is determined according to leaching solution temperature, pressure, mineralogical composition, leaching solution composition, and is of the present invention:
Molten soaking the time: 4-10 hour;
Leaching solution flow velocity: 150-250ml/ minute;
Leaching solution flow: 0.8-1.2m
3/ hour;
Leaching solution goes out halogen amount: 200-450m
3/ hour.
The thick potassium that described crystallization goes out is in rinse bath, by thick potassium: fresh water=1: 0.3, add water and wash, separate solid, liquid mutually after, high-quality Repone K, the water after the washing returns potassium-rich brine and recycles.
Amount of water in the washing is pressed the column count formula and is drawn:
In the formula: W
2Thick potassium washing actual used water amount (ton)
Q
2Thick potassium weight (ton)
M
2Thick potassium sodium chloride-containing amount (ton/ton)
M
2Sodium-chlor fills content (ton/ton) perhaps in the smart potassium
M
3Thick potassium contains magnesium chloride amount (ton/ton)
M
3Magnesium chloride fills content (ton/ton) perhaps in the smart potassium
t
2Wash temperature (℃)
N
2Thick potassium water content (ton/ton).
The fast decomposition and crystallization water consumption of described control is calculated by following formula:
In the formula: W
1Carnallitite decomposes actual used water amount (ton)
Q
1Carnallitite weight (ton)
M
1Content of magnesium chloride in the carnallitite (ton/ton)
N
1Water content in the carnallitite (ton/ton)
T
1The separation temperature of decomposition course (℃).
Described crystallisation by cooling is divided into one section cooling, two sections coolings, and equipment used is the two-stage vacuum crystallizer, and is aided with naturally cooling means such as cold crystallization, air cooling.
Described evaporative crystallization adopts based on the multiple-effect forced circulation evaporation, and solar heating is the type of heating of assisting.
In the described production by dissolving and leaching process, the requirement of each composition of leaching solution is: KCl content is low more, and then the KCl amount is just many more in the potassium-rich brine of extraction, and benefit is high more; It is saturated or closely saturated that NaCl content should keep, so that not extraction or few extraction NaCl; MgCl
2Content should be near KCl, NaCl and KClMgCl
26H
2MgCl when O three salt are total to saturation point
2Amount is so that effectively control MgCl
2Produced quantity.
The present invention compared with prior art has following advantage and effect:
1, the leaching solution with the present invention preparation carries out selectivity production by dissolving and leaching process solid sylvite ore, makes useful Repone K mineral dissolving enter that liquid phase gets rich potassium saltwater brine and by extraction, and the Repone K recovery ratio is higher, and cost is lower.Unwanted impure mineral then original place stays, and neither produces waste liquid and refuse, does not destroy the face of land and vegetation thereof again, helps increasing economic efficiency and preserving the ecological environment;
2, pass through the organic and ingenious combination of multi-component crystallization technology, not only can give full play to the characteristic and the advantage of various crystallization processes, and can reclaim the Repone K of valency repeatedly, and obtain to be convenient to high-quality, the coarsness Repone K product of deep processing, effectively improve the product yield, cut down the consumption of energy;
3, the saline solution of crystallisation process generation is mixed with leaching solution re-injection ore body circulation exploitation again, and waste water then returns rich potassium saltwater brine and recycles, thereby does not discharge any waste water and refuse, in free from environmental pollution, effectively reduces production cost.
Description of drawings
Fig. 1 is the present invention's process flow sheet.
Embodiment
Below by embodiment the present invention is described in detail.
Embodiment
Ore with Laos's everything sylvite ore is a raw material, and its industrial scale is for producing 100000 tons of Repone K per year.The ore main chemical compositions:
KCl 7.61-22.26%, average 15.70%, MgCl
20.53-28.36%, average 21.48%, NaCl 20-30%, Br 0.2-0.3%.
Mineral composition: be mainly carnallitite (KClMgCl
26H
2O), sylvite (KCl, NaCl), bischofite (MgCl
26H
2O), a small amount of tachyhydrite (CaCl
2MgCl
212H
2O).
Adopt that twin-well is molten to soak the method exploitation, arrange that in first exploiting field centre hole 225mm drilling well two is to (4 mouthfuls), to constitute a productive unit:
1, production by dissolving and leaching process process condition:
Leaching solution chemical composition (weight percent):
Repone K 0.1%
Sodium-chlor 2%
Magnesium chloride 25%
Surplus is abraum salt liquid and water;
Leaching solution temperature: 45 ℃;
Leaching solution flow: 5m
3/ minute;
Molten soaking the time: 6 hours;
Molten compregnate power: 1 meter of the every decline of hole depth, required surface pressure is 0.115kg/cm
2, press the 300m hole-depth gauge, be 34.7Kg/cm
2
Leaching solution went out halogen amount: 300m3/ hour;
Leach liquor (rich potassium saltwater brine) chemical ingredients: KCl 4.18%, MgCl
226.6%, NaCl 2%;
2, crystallisation step:
2.1, the rich potassium saltwater brine of extraction is sent into multiple-effect evaporator, adopt the quadruple effect pump circulation to carry out evaporative crystallization, its processing parameter sees Table 1, its temperature is 100 ℃, vaporize water returns the leaching solution pond; Crystallization precipitate gets the high temp. salt of sodium chloride-containing and analyses the salt mother liquor after sedimentation, centrifugation, and high temp. salt returns molten soaking pit preparation leaching solution, analyses the salt mother liquor and sends to crystallisation by cooling;
2.2, under 30 ℃ of temperature condition, carry out crystallisation by cooling, to analyse the salt mother liquor sends in the two-stage vacuum cooling crystallizer, cooling, cooling, make refrigerant with underground water, the crystallisation by cooling processing parameter sees Table 2, table 3, cold analysis low-sodium carnalite composition: KCl/NaCl 〉=5%, NaCl≤5%, the old halogen composition of isolating behind the low-sodium carnalite is; MgCl
2〉=34.5%;
2.3, under 15-40 ℃, normal pressure, control fast decomposition and crystallization, by charge ratio be: carnallitite: water: convert halogen carnallitite=1: 0.5: 5, average rate adds the decomposition and crystallization reactor with carnallitite, control stirring velocity 80rpm, 80 minutes crystallization reaction time, thick potassium is separated out in crystallization, after isolating thick potassium with centrifuge separator, decomposition nut liquid, thick potassium composition is: KCl 〉=84%, NaCl5%, MgCl
23.6%, mean particle size 0.5mm, the decomposition nut liquid composition is: KCl 3%, and NaCl 2.3%, MgCl
224.5%, control fast decomposition and crystallization processing parameter and see Table 4;
2.4, the decomposition nut liquid average rate of the old halogen of 2 steps and 3 steps added to convert converts the halogen crystallization in the halogen crystallizer, control stirring velocity 200rpm in 50 minutes reaction times, converts halogen and compares M
25: F=1: 2, further the Repone K composition crystallization in old halogen and the decomposition nut liquid is separated out, get the carnallitite slip and convert the halogen mother liquor, the carnallitite composition is: KCl/NaCl 〉=4%, NaCl≤5%, median size .0.7mm, converting the halogen mother liquor composition is: KCl 0.2%, and NaCl 0.7%, MgCl
231%,
Convert the halogen mother liquor and return molten soaking pit preparation leaching solution, convert the halogen carnallitite and send 3 steps to control fast decomposition and crystallization to go out thick potassium, convert the halogen technology parameter and see Table 5;
2.5, will return molten soaking pit vaporize water, high temp. salt, convert the halogen mother liquor and be used for being mixed with and be recycled into ore body behind the leaching solution and carry out the selectivity exploitation;
2.6, the thick potassium that goes out of crystallization is in rinse bath, by thick potassium: fresh water=1: 0.3, add water and wash, separate solid, liquid mutually after, high-quality Repone K, its product composition is: KCl 98%, NaCl 1%, MgCl
20.3%, median size 0.35mm, the water after the washing returns potassium-rich brine and recycles, and thick potassium washing process parameter sees Table 6.
Table 1 quadruple effect forced circulation evaporation design variable
| Project | Unit | One imitates | Two imitate | Triple effect | Quadruple effect | ||||
| Heating chamber | Evaporator room | Heating chamber | Evaporator room | Heating chamber | Evaporator room | Heating chamber | Evaporator room | ||
| The steam absolute pressure | MPa | 0.393 | 0.18 | 0.18 | 0.08 | 0.078 | 0.034 | 0.033 | 0.01 |
| Vapor temperature | ℃ | 143 | 117.7 | 117.2 | 93 | 92.7 | 70 | 69 | 45.4 |
| Feed liquid boiling point liter | ℃ | 11.5 | 10 | 8.5 | 6.5 | ||||
| Feed liquid is temperature eventually | ℃ | 129.2 | 103.7 | 78.5 | 52.9 | ||||
| The pipeline temperature difference loss | ℃ | 0.5 | 1 | 1 | 1 | ||||
| Effective temperature difference | ℃ | 11.3 | 11 | 11.7 | 13.6 | ||||
| Thermosteresis | ℃ | 2.5 | 2.5 | 2.5 | 2.5 | ||||
| Heat transfer coefficient | Kcal/ m 2℃h | 1950 | 1800 | 1650 | 1500 | ||||
One section carnallitite crystallisation by cooling of table 2 design variable
| Project | Unit | The one-level vacuum cyrsytalliser |
| The secondary steam absolute pressure | MPa | -0.08 |
| Steam temperature | ℃ | 54 |
| The feed liquid boiling point rises | ℃ | 11 |
| Feed liquid is temperature eventually | ℃ | 65 |
Two sections low thermohaline crystallisation by cooling design variables of table 3
| Project | Unit | The secondary vacuum cyrsytalliser |
| The secondary steam absolute pressure | MPa | -0.099 |
| Steam temperature | ℃ | 19 |
| The feed liquid boiling point rises | ℃ | 11 |
| Feed liquid is temperature eventually | ℃ | 30 |
The fast decomposition and crystallization technology main design parameters of table 4 control
| Project | Unit | Processing parameter | Remarks |
| The carnallitite dosage | t/h | 84.57 | |
| The carnallitite quality | KCl/NaCl≥5，NaCl≤5％ | ||
| Charge ratio | Car∶H 2O∶M 25＝1∶0.5∶4～6 | * | |
| The reactor stirring velocity | rpm | 50～100 | |
| The residence time | min | 60～90 | |
| Underflow magma concentration | ％ | 18～25 | |
| Thick potassium quality product | KCl≥84％ |
Table 5 is converted halogen crystallization processes main design parameters
| Project | Unit | Processing parameter | Remarks |
| Convert the halogen ratio | M 25∶F≈1∶2 | ||
| The carnallitite quality | KCl/NaCl≥5，NaCl≤5％ | ||
| The reactor stirring velocity | rpm | 5～100 | |
| The residence time | min | 60 | |
| Underflow magma concentration | ％ | 18～25 |
The thick potassium washing process main design parameters of table 6
| Project | Unit | Processing parameter | Remarks |
| The washing amount of water | Thick potassium: fresh water ≈ 1: 0.3 | * | |
| Smart potassium quality | KCl (butt) 〉=98% | ** | |
| Stirring velocity | rpm | 50～100 | |
| The residence time | min | 3～10 | |
| Starch concentration again | ％ | 18～35 |
Claims (1)
1, a kind of solid ore deposit production by dissolving and leaching process-multi-component crystallization is produced the method for Repone K, and it comprises the selectivity production by dissolving and leaching process, and the potassium-rich brine evaporative crystallization that will exploitation comes out, and it is characterized in that:
The used leaching solution of selectivity production by dissolving and leaching process is made up of the chemical composition of following weight percent:
Repone K≤0.4%
Sodium-chlor 1.8-2%
Magnesium chloride 24.5-26%
Surplus is abraum salt liquid and water;
Leaching solution temperature: 25-60 ℃;
Leaching solution flow velocity: 150-250ml/ minute;
Leaching solution flow: 0.8-1.2m
3/ hour;
Molten soaking the time: 4-10 hour;
Molten compregnate power: 1 meter of the every decline of hole depth, required surface pressure is 0.115kg/cm
2
Leaching solution goes out halogen amount: 200-450m
3/ hour;
The rich potassium saltwater brine that exploitation is come out is directly through following crystallization processes step:
A, under 30-145 ℃ of temperature condition, based on the multiple-effect forced circulation evaporation, solar heating is that the mode of assisting is carried out evaporative crystallization, vaporize water returns the leaching solution pond; Crystallization precipitate through separate sodium chloride-containing high temp. salt and analyse the salt mother liquor, high temp. salt returns molten soaking pit;
B, under 20-40 ℃ of temperature condition, the above-mentioned salt mother liquor of analysing is carried out one section, two sections crystallisation by cooling, and is aided with cold crystallization, air cooling, separate out low-sodium carnalite, isolate low-sodium carnalite after, obtaining main component is the old halogen of magnesium chloride;
C, under 15-40 ℃ of temperature condition, feed intake by following weight ratio: carnallitite: water: convert halogen carnallitite=1: 0.5: 4-6, control fast decomposition and crystallization, control stirring velocity 50-100rpm, 60-90 minute crystallization reaction time, isolate thick potassium after, decomposition nut liquid;
D, the old halogen of B step and the decomposition nut liquid of C step are converted the halogen crystallization, control stirring velocity 100-300rpm reaction times 30-70 minute, converts halogen and compares M
25: F=1: 2, crystallization gets carnallitite slip and convert the halogen mother liquor, converts the halogen mother liquor and returns molten soaking pit, and the carnallitite slip returns the C step again to be controlled fast decomposition and crystallization and goes out thick potassium;
The thick potassium that E, crystallization go out, by thick potassium: fresh water=1: 0.3, add water and wash, separate solid, liquid mutually after, high-quality Repone K, the water after the washing returns potassium-rich brine and recycles;
F, the vaporize water that will return molten soaking pit, high temp. salt, convert the halogen mother liquor and be mixed with to be recycled into behind the leaching solution and carry out the selectivity exploitation in the ore body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021339163A CN1304293C (en) | 2002-10-15 | 2002-10-15 | Preparation of potassium chloride by multi-component crystallization of solid mineral production by dissolving and leaching process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021339163A CN1304293C (en) | 2002-10-15 | 2002-10-15 | Preparation of potassium chloride by multi-component crystallization of solid mineral production by dissolving and leaching process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1490246A CN1490246A (en) | 2004-04-21 |
| CN1304293C true CN1304293C (en) | 2007-03-14 |
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ID=34145713
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|---|---|---|---|
| CNB021339163A Expired - Fee Related CN1304293C (en) | 2002-10-15 | 2002-10-15 | Preparation of potassium chloride by multi-component crystallization of solid mineral production by dissolving and leaching process |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462743B (en) * | 2007-12-17 | 2010-10-13 | 贵阳铝镁设计研究院 | Method for preparing low sodium low potassium content carnallite |
| CN102491373B (en) * | 2011-12-22 | 2013-08-14 | 化工部长沙设计研究院 | Method for producing potassium chloride, sodium chloride and magnesium sheet from bittern extracted from carnallite mine |
| CN103253685B (en) * | 2013-03-04 | 2014-12-17 | 云南省化工研究院 | Method for producing industrial potassium chloride through hot melting crystallization of underground embedded solid potassium salt mine |
| CN106830014B (en) * | 2017-03-07 | 2018-08-28 | 青海省矿业集团股份有限公司 | Leachant based on high strong brine in coal chemical industry |
| CN111087060A (en) * | 2019-12-31 | 2020-05-01 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for recovering potassium chloride from fluoride-containing wastewater and recycling wastewater |
| CN111533138B (en) | 2020-05-06 | 2022-08-26 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride by utilizing carnallite |
| CN111362730B (en) * | 2020-05-06 | 2021-11-02 | 中国科学院青海盐湖研究所 | Method for preparing low-sodium carnallite and potassium chloride by using high-sodium carnallite |
| CN112340753B (en) * | 2020-11-23 | 2022-11-08 | 青海盐湖工业股份有限公司 | Method and system for recycling potassium chloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032149A (en) * | 1987-09-24 | 1989-04-05 | 全苏制盐科学研究设计院 | From contain the potassium raw material, obtain the method that concentrates Repone K |
| CN1063663A (en) * | 1992-03-05 | 1992-08-19 | 化学工业部化工矿山设计研究院 | Potassium chloride preparing by chloride type patassium brine |
-
2002
- 2002-10-15 CN CNB021339163A patent/CN1304293C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032149A (en) * | 1987-09-24 | 1989-04-05 | 全苏制盐科学研究设计院 | From contain the potassium raw material, obtain the method that concentrates Repone K |
| CN1063663A (en) * | 1992-03-05 | 1992-08-19 | 化学工业部化工矿山设计研究院 | Potassium chloride preparing by chloride type patassium brine |
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|---|---|
| CN1490246A (en) | 2004-04-21 |
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