CN110607460B - Method for extracting potassium from potassium-containing rock - Google Patents
Method for extracting potassium from potassium-containing rock Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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Abstract
The invention belongs to the technical field of potassium-containing rock treatment, and particularly relates to a method for extracting potassium from potassium-containing rock, which comprises the following steps: 1) primary calcination; 2) and (3) cooling: cooling the primary calcined product to room temperature; 3) ultrasonic reaction: mixing the cooled product with an acid solution, placing the mixture in an ultrasonic reaction kettle, controlling the temperature of the material to be 80-100 ℃ for reaction, and carrying out solid-liquid separation after the reaction to obtain a solid; 4) microwave reaction: mixing the ultrasonic reaction product with an auxiliary agent, and placing the mixture in a microwave reaction kettle to react at the temperature of 120 ℃ and 130 ℃; 5) secondary calcination; the method has the characteristics of improving the dissolution rate and activity of potassium, can treat various potassium-containing rocks, reduces sewage discharge and heat energy consumption, and shortens treatment time.
Description
Technical Field
The invention belongs to the technical field of potassium-containing rock treatment, and particularly relates to a method for extracting potassium from potassium-containing rock.
Background
The soluble potassium ore resources in China are deficient and are distributed extremely unevenly, but the reserves of the insoluble potassium-containing rock resources in China are large, so that the effective utilization of the insoluble potassium-containing rock resources is of research significance. According to the utilization process of the water-insoluble clock-containing rock, the utilization method can be divided into three parts:
firstly, the potassium-containing rock is directly applied to farmlands after being ground, but the method has large resource waste, and effective resources cannot be fully utilized;
secondly, a high-temperature roasting method: preparing slow-release potash fertilizer by a fire method: directly mixing potassium feldspar with auxiliary agents such as dolomite, limestone and the likeMixing, sintering at high temperature to produce citrate soluble potassium-calcium fertilizer and silicon compound fertilizer; for example, the phosphorus-potassium composite fertilizer is prepared by calcining serpentine or dolomite for phosphorus-potassium mine as an auxiliary agent at the temperature of 1400 ℃ and 1500 ℃, after the citrate-soluble potassium fertilizer is applied to soil, the citrate-soluble potassium fertilizer is slowly dissolved by organic acid secreted by the roots of plants, and is absorbed by the plants through ion exchange, so that nutrient elements are not easily leached and lost, and are not easily fixed by other compounds in the soil. Respectively grinding potassium feldspar and limestone into fine powder, mixing according to equal proportion, fully mixing, preparing into massive raw material, drying, sintering the dried raw material block in a high-temperature furnace at 1200 ℃ for 30min, wherein the potassium dissolution rate can reach more than 97.1 percent, and citric acid soluble potassium produced by the method can be slowly and completely dissolved out and absorbed by plants; ② sintering method. Korea Chilobrachys and the like utilize CaCl2The potassium feldspar serving as an additive is sintered with the potassium feldspar, so that the reaction temperature is obviously reduced, the sintering temperature is 900 ℃ at most, and the potassium dissolution rate is over 90-95%; however, the high-temperature roasting method has low utilization rate of potassium because the product produced by the method is citrate soluble potassium, and because elements such as silicon, aluminum, iron and the like in potassium-containing rocks remain in the fertilizer, the elements cannot be absorbed by plants and are easy to cause desertification of soil, the application of the potassium fertilizer produced by the method is greatly limited.
Thirdly, a wet chemical method: firstly, a pressure heating method: various leaching agents are used for decomposing potassium feldspar to prepare soluble potassium salt at the temperature of 150-500 ℃ and under the pressure of 0.3-6.1MPa, but the pressure is large, the investment cost is high, and the industrialization is difficult; ② a thermal decomposition water immersion method: the method comprises the steps of carrying out thermal decomposition reaction on potassium feldspar and an auxiliary agent at the temperature of 600-1200 ℃ to generate water-soluble potassium salt, and then adding water to extract and separate the potassium salt. Common auxiliary agents are fluoride, CaO and CaCO3、CaSO4Soda ash, caustic soda, etc.; qiulong et al uses potassium feldspar (7.5%) and apatite (10.25%) and mixes them, and uses wet extraction to remove water from the apatite, then adds CaCO3And a small amount of additive, thermally decomposing for 2h at 900-950 ℃, and leaching potassium sulfate with water, wherein the potassium decomposition rate can reach 90-93%; through analysis, the composition of the residue is similar to that of cement clinker, and the residue can be directly used as cement; mixing insoluble potassium-containing rock with sodium carbonate or sodium hydroxide at a certain ratio, and treating at 850 deg.C and 750-Sintering at a warm temperature, taking caustic soda as a material, and performing hydrothermal extraction at 98 ℃ to prepare potassium carbonate suitable for the production of the electronic industry; but the wet chemical method has serious raw material waste, long production period and difficult discharge of byproduct sewage.
Patent No. CN201610907570.8 discloses a method for preparing a low-silicon X-type molecular sieve by melting and activating potassium-containing rock with NaCO-NaOH mixed alkali, but the method has strict requirements on the contents of potassium oxide, silicon oxide, aluminum oxide, sodium oxide and ferrous oxide in the potassium-containing rock, so that the components of a treated object need to be detected during treatment, and the control difficulty is high.
Disclosure of Invention
The invention provides a method for extracting potassium from potassium-containing rocks to solve the technical problems.
The method is realized by the following technical scheme:
a method for extracting potassium from potassium-containing rocks comprises the following steps:
1) primary calcination: crushing the potassium-containing rock to 80-200 meshes according to the weight ratio of the potassium-containing rock: bone meal: carbon powder is 100: (1-3) adding bone meal and carbon powder in the proportion of (21-23), and calcining for 0.5-1h at the temperature of 600-;
2) and (3) cooling: cooling the primary calcined product to room temperature;
3) ultrasonic reaction: and (3) mixing the cooled product with an acid solution according to a solid-to-liquid ratio of 1: (1.2-1.5), placing the mixture in an ultrasonic reaction kettle, controlling the material temperature to be 80-100 ℃ to react for 30-50min, and carrying out solid-liquid separation after the reaction to obtain a solid;
4) microwave reaction: mixing the ultrasonic reaction product and an auxiliary agent according to a solid-liquid ratio of 1: (1.3-1.7), placing the mixture in a microwave reaction kettle, controlling the material temperature to be 120-130 ℃, and reacting for 30-50 min;
5) secondary calcination: the microwave reaction product is placed in a kiln and calcined for 60-120min at the temperature of 300-500 ℃.
The carbon powder is activated for 2-3h at the ball mill rotation speed of 500-600r/min and the temperature of 60-80 ℃ and then taken out.
The potassium-containing rock is composed of the following raw materials in parts by weight: 5-10 parts of illite, 3-8 parts of leucite, 11-16 parts of nepheline, 20-25 parts of muscovite, 4-9 parts of sericite, 30-40 parts of alunite and 50-60 parts of potassium feldspar.
The power of the ultrasonic wave is 700-900w, and the frequency is 25-29 kHz.
The acid solution is a hydrochloric acid solution with the concentration of 30-50%.
The auxiliary agent comprises the following raw materials in parts by weight: 3-7 parts of calcium chloride, 1-5 parts of sodium carbonate, 6-10 parts of sodium chloride and 10-15 parts of tartaric acid.
The microwave power is 5-15 kw.
Has the advantages that:
from the mineralogical perspective, common water-insoluble potassium-containing rocks mainly comprise potash feldspar, biotite, leucite, illite, glauconite, alunite and the like, and the molecular formulas and the potassium oxide contents of various water-insoluble potassium-containing rocks are shown in table 1:
TABLE 1
By utilizing various minerals with different structures, the minerals can be mutually activated by utilizing the characteristics of different structures and different component contents, so that the migration of metal ions is improved; the application utilizes the bone meal and the carbon powder to improve the melting characteristic of the minerals, so that the soluble potassium is quickly dissolved out.
The invention utilizes the ultrasonic effect to change the mineral structure, combines tartaric acid as a crystal modifier, and coordinates the exchange effect of calcium chloride, sodium carbonate and sodium chloride to fully dissolve soluble potassium to change partial insoluble potassium, utilizes the microwave treatment and the acid action to activate components such as potassium, silicon, aluminum and the like in the mineral, and finally combines the calcination treatment to further dissolve the potassium, and utilizes the liquid gasification effect to improve the activity of the dissolved potassium, thereby improving the utilization rate of the potassium.
In conclusion, the method has the characteristics of improving the dissolution rate and activity of potassium, can treat various potassium-containing rocks, reduce sewage discharge and heat energy consumption, shorten the total treatment time, is simple and easy to control, and reduces the calcination temperature and time.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A method for extracting potassium from potassium-containing rocks comprises the following steps:
1) primary calcination: crushing the potassium-containing rock to 200 meshes according to the weight ratio of the potassium-containing rock: bone meal: carbon powder is 100: adding bone meal and carbon powder in a ratio of 3:23, and calcining for 1h at the temperature of 700 ℃;
2) and (3) cooling: cooling the primary calcined product to room temperature;
3) ultrasonic reaction: and (3) mixing the cooled product with an acid solution according to a solid-to-liquid ratio of 1: 1.5, placing the mixture in an ultrasonic reaction kettle, controlling the material temperature to be 100 ℃ to react for 50min, and carrying out solid-liquid separation after the reaction to obtain a solid;
4) microwave reaction: mixing the ultrasonic reaction product and an auxiliary agent according to a solid-liquid ratio of 1: 1.7, placing the mixture in a microwave reaction kettle, and controlling the material temperature to be 130 ℃ to carry out reaction for 50 min;
5) secondary calcination: placing the microwave reaction product in a kiln, and calcining for 120min at the temperature of 500 ℃;
the carbon powder is activated for 2 to 3 hours at the rotating speed of 600r/min and the temperature of 80 ℃ in the ball mill and then taken out;
the potassium-containing rock is composed of the following raw materials: 10kg of illite, 8kg of leucite, 16kg of nepheline, 25kg of muscovite, 9kg of sericite, 40kg of alunite and 60kg of potash feldspar;
the power of the ultrasonic wave is 900w, and the frequency is 29 kHz;
the acid solution is 50% hydrochloric acid solution;
the auxiliary agent consists of the following raw materials: 7kg of calcium chloride, 5kg of sodium carbonate, 10kg of sodium chloride and 15kg of tartaric acid;
the microwave power is 15 kw.
Example 2
A method for extracting potassium from potassium-containing rocks comprises the following steps:
1) primary calcination: crushing the potassium-containing rock to 80 meshes according to the weight ratio of the potassium-containing rock: bone meal: carbon powder is 100: adding bone powder and carbon powder at a ratio of 1:21, and calcining at 600 deg.C for 0.5 h;
2) and (3) cooling: cooling the primary calcined product to room temperature;
3) ultrasonic reaction: and (3) mixing the cooled product with an acid solution according to a solid-to-liquid ratio of 1: 1.2, placing the mixture in an ultrasonic reaction kettle, controlling the temperature of the material to be 80 ℃ for reaction for 30min, and carrying out solid-liquid separation after the reaction to obtain a solid;
4) microwave reaction: mixing the ultrasonic reaction product and an auxiliary agent according to a solid-liquid ratio of 1: 1.3, placing the mixture in a microwave reaction kettle, and controlling the material temperature to be 120 ℃ to carry out reaction for 30 min;
5) secondary calcination: placing the microwave reaction product in a kiln, and calcining for 60min at the temperature of 300 ℃;
the carbon powder is activated for 2 hours at the rotating speed of 500r/min and the temperature of 60 ℃ in the ball mill and then taken out;
the potassium-containing rock is composed of the following raw materials: 5kg of illite, 3kg of leucite, 11kg of nepheline, 20kg of muscovite, 4kg of sericite, 30kg of alunite and 50kg of potash feldspar;
the power of the ultrasonic wave is 700w, and the frequency is 25 kHz;
the acid solution is a hydrochloric acid solution with the concentration of 30%;
the auxiliary agent consists of the following raw materials: 3kg of calcium chloride, 1kg of sodium carbonate, 6kg of sodium chloride and 10kg of tartaric acid;
the microwave power is 5 kw.
Example 3
A method for extracting potassium from potassium-containing rocks comprises the following steps:
1) primary calcination: crushing the potassium-containing rock to 100 meshes according to the weight ratio of the potassium-containing rock: bone meal: carbon powder is 100: adding bone meal and carbon powder in a ratio of 2:22, and calcining for 0.8h at the temperature of 650 ℃;
2) and (3) cooling: cooling the primary calcined product to room temperature;
3) ultrasonic reaction: and (3) mixing the cooled product with an acid solution according to a solid-to-liquid ratio of 1: 1.3, placing the mixture in an ultrasonic reaction kettle, controlling the material temperature to be 90 ℃ for reaction for 40min, and carrying out solid-liquid separation after the reaction to obtain a solid;
4) microwave reaction: mixing the ultrasonic reaction product and an auxiliary agent according to a solid-liquid ratio of 1: 1.5, placing the mixture in a microwave reaction kettle, and controlling the material temperature to 125 ℃ to carry out reaction for 40 min;
5) secondary calcination: placing the microwave reaction product in a kiln, and calcining for 90min at the temperature of 400 ℃;
the carbon powder is activated for 2.5 hours at the rotating speed of 550r/min and the temperature of 70 ℃ in the ball mill and then taken out;
the potassium-containing rock is composed of the following raw materials: 8kg of illite, 5kg of leucite, 13kg of nepheline, 22kg of muscovite, 7kg of sericite, 35kg of alunite and 55kg of potash feldspar;
the power of the ultrasonic wave is 800w, and the frequency is 27 kHz;
the acid solution is a hydrochloric acid solution with the concentration of 40%;
the auxiliary agent consists of the following raw materials: 5kg of calcium chloride, 3kg of sodium carbonate, 8kg of sodium chloride and 12kg of tartaric acid;
the microwave power is 10 kw.
Comparative example 1
The difference from example 3 is that: tartaric acid is not added in the auxiliary agent.
Comparative example 2
The difference from example 3 is that: the carbon powder was not activated.
Comparative example 3
The difference from example 3 is that: firstly carrying out microwave reaction and then carrying out ultrasonic reaction.
The extraction rates of potassium and aluminum in examples 1-3 and comparative examples 1-3 are shown in table 1:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Percentage of potassium dissolution/%) | 98.5 | 98.2 | 99.1 | 90.3 | 92.6 | 97.4 |
| Aluminum dissolution rate/%) | 95.7 | 94.8 | 96.1 | 87.3 | 90.2 | 91.6 |
Claims (4)
1. The method for extracting potassium from potassium-containing rocks is characterized by comprising the following steps of:
1) primary calcination: crushing the potassium-containing rock to 80-200 meshes according to the weight ratio of the potassium-containing rock: bone meal: carbon powder is 100: (1-3) adding bone meal and carbon powder in the proportion of (21-23), and calcining for 0.5-1h at the temperature of 600-;
2) and (3) cooling: cooling the primary calcined product to room temperature;
3) ultrasonic reaction: and (3) mixing the cooled product with an acid solution according to a solid-to-liquid ratio of 1: (1.2-1.5), placing the mixture in an ultrasonic reaction kettle, controlling the material temperature to be 80-100 ℃ to react for 30-50min, and carrying out solid-liquid separation after the reaction to obtain a solid;
4) microwave reaction: mixing the ultrasonic reaction product and an auxiliary agent according to a solid-solid ratio of 1: (1.3-1.7), placing the mixture in a microwave reaction kettle, controlling the material temperature to be 120-130 ℃, and reacting for 30-50 min;
5) secondary calcination: placing the microwave reaction product in a kiln, and calcining for 60-120min at the temperature of 300-500 ℃;
the potassium-containing rock is composed of the following raw materials in parts by weight: 5-10 parts of illite, 3-8 parts of leucite, 11-16 parts of nepheline, 20-25 parts of muscovite, 4-9 parts of sericite, 30-40 parts of alunite and 50-60 parts of potassium feldspar;
the auxiliary agent comprises the following raw materials in parts by weight: 3-7 parts of calcium chloride, 1-5 parts of sodium carbonate, 6-10 parts of sodium chloride and 10-15 parts of tartaric acid;
the acid solution is a hydrochloric acid solution with the concentration of 30-50%.
2. The method as claimed in claim 1, wherein the carbon powder is activated at a ball mill rotation speed of 500-600r/min and a temperature of 60-80 ℃ for 2-3h and then taken out.
3. The method for extracting potassium from potassium-containing rock as claimed in claim 1, wherein the power of the ultrasonic wave is 700-900w, and the frequency is 25-29 kHz.
4. The method for extracting potassium from potassium-containing rocks according to claim 1, wherein the microwave power is 5 to 15 kw.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104388668A (en) * | 2014-10-30 | 2015-03-04 | 北京矿冶研究总院 | Method for acid-alkali combined extraction of aluminum, potassium and sodium from water-insoluble potassium ore |
| CN105084395A (en) * | 2015-08-05 | 2015-11-25 | 铜仁市万山区盛和矿业有限责任公司 | Method for producing soluble potassium through potassium feldspar |
| CN105883830A (en) * | 2016-04-07 | 2016-08-24 | 陕西大秦钾业有限公司 | Method for preparing kaliophilite by conducting microwave activation on potassium feldspar and kaliophilite prepared through method |
| CN105884406A (en) * | 2014-12-15 | 2016-08-24 | 天津城建大学 | Method for low-temperature extraction of potassium in water-insoluble potassium-containing ore |
| CN106219578A (en) * | 2016-07-22 | 2016-12-14 | 中国科学院青海盐湖研究所 | A kind of preparation method of water solublity potassium salt |
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- 2019-09-16 CN CN201910871678.XA patent/CN110607460B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388668A (en) * | 2014-10-30 | 2015-03-04 | 北京矿冶研究总院 | Method for acid-alkali combined extraction of aluminum, potassium and sodium from water-insoluble potassium ore |
| CN105884406A (en) * | 2014-12-15 | 2016-08-24 | 天津城建大学 | Method for low-temperature extraction of potassium in water-insoluble potassium-containing ore |
| CN105084395A (en) * | 2015-08-05 | 2015-11-25 | 铜仁市万山区盛和矿业有限责任公司 | Method for producing soluble potassium through potassium feldspar |
| CN105883830A (en) * | 2016-04-07 | 2016-08-24 | 陕西大秦钾业有限公司 | Method for preparing kaliophilite by conducting microwave activation on potassium feldspar and kaliophilite prepared through method |
| CN106219578A (en) * | 2016-07-22 | 2016-12-14 | 中国科学院青海盐湖研究所 | A kind of preparation method of water solublity potassium salt |
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