CN103172410A - Method for extracting potassium from potassium-containing shale - Google Patents
Method for extracting potassium from potassium-containing shale Download PDFInfo
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- CN103172410A CN103172410A CN2011104379263A CN201110437926A CN103172410A CN 103172410 A CN103172410 A CN 103172410A CN 2011104379263 A CN2011104379263 A CN 2011104379263A CN 201110437926 A CN201110437926 A CN 201110437926A CN 103172410 A CN103172410 A CN 103172410A
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Abstract
The invention discloses a method for extracting potassium from a potassium-containing shale. The method comprises the following steps of: taking the potassium-containing shale, grinding, mixing the ground potassium-containing shale with anhydrous calcium chloride, calcining at the temperature of 600-1,000 DEG C, cooling to room temperature, extracting by using an extracting agent, and filtering to obtain a filtrate which is a potassium extract. Because the anhydrous calcium chloride is used as a fluxing agent, the reaction of molten cations is accelerated. The whole method is simple, is short in reaction period, can be used for effectively extracting the non-soluble potassium from the potassium-containing shale and can ensure that the potassium extraction rate is 90%. The obtained potassium extract can be directly used for preparing a nitrogen-phosphorus-potassium compound fertilizer and meets the low-concentration index specified in the national standard GB15063-2009 of the compound fertilizer. The potassium extract contains more than 4% of potassium. The problem on the shortage of potassium fertilizer in China is solved.
Description
Technical field
The present invention relates to the extractive technique field of potassium, particularly relate to a kind of method of extracting potassium from potassium-bearing shale.
Background technology
Potash fertilizer is a kind of very important material used for agriculture, and the traditional method of producing potash fertilizer is to utilize the soluble potassium salt mineral to extract potassium to prepare potash fertilizer, or directly utilizes the sylvite mineral to prepare potash fertilizer for raw material, and China is a large agricultural country, the potash fertilizer supply shortage.
At present the present situation of China's potassium ore resources is: solubility extremely scarce, but the reserves of insoluble are very abundant.The refractory potassic mine resource is mainly potassium-bearing shale, and extracting at present potassium from potassium-bearing shale is mainly to process through physics and chemistry, and the non-dissolubility potassium in potassium-bearing shale is converted into soluble potassium, then adopts leaching agent to extract.Present extracting method is only applicable to potassium felspar sand mostly, and extraction cost is high.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes the more difficult extraction of potassium from potassium-bearing shale, a kind of method of extracting potassium from potassium-bearing shale is provided, technique is simple, and gained potassium leach liquor can directly be used for preparing nitrogen-phosphorus-potassium compound fertilizer, solves the problem of China's potash fertilizer shortage.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
The present invention extracts the method for potassium from potassium-bearing shale: get potassium-bearing shale, pulverize rear and Calcium Chloride Powder Anhydrous mixing, 600-1000 ℃ of lower roasting, be cooled to room temperature, use leaching agent H
0Leach, after filtering, filtrate is the potassium leach liquor, wherein leaching agent H
0That mass percentage concentration is the H of 1-10%
2O
2The aqueous solution.Preparation H
2O
2The aqueous solution can select purity less than 30% H
2O
2
Further, the above-mentioned method of extracting potassium from potassium-bearing shale is: get potassium-bearing shale, pulverize rear and Calcium Chloride Powder Anhydrous mixing, at 700-900 ℃ of lower roasting 50-70min, be cooled to room temperature, use leaching agent H
0Lixiviate 50-70min filters, and filtrate is the potassium leach liquor, wherein leaching agent H
0That mass percentage concentration is the H of 4-8%
2O
2The aqueous solution.
Further, in the aforementioned method of extracting potassium from potassium-bearing shale, potassium-bearing shale is crushed to granularity be-0.07～-0.08mm, preferably potassium-bearing shale is divided to be crushed to granularity and to be-0.074mm.The weight ratio of potassium-bearing shale and Calcium Chloride Powder Anhydrous is 1:1-2, and preferred weight part ratio is 1:1.5.
In preceding method, add phosphoric acid and ammoniacal liquor in the potassium leach liquor, the fully rear filtering drying of solution crystallization had both got nitrogen-phosphorus-potassium compound fertilizer.The usage ratio of potassium ion, phosphoric acid, ammoniacal liquor adopts the ratio of this area routine, and the concentration of phosphoric acid and ammoniacal liquor and consumption are decided by the volume of potassium leach liquor and the content of potassium.Along with the increase of potassium-bearing shale sample ore consumption, in gained potassium leach liquor, the content of potassium also increases thereupon, and after adding appropriate certain density phosphoric acid and ammoniacal liquor, in products obtained therefrom, the content of potassium also increases.
In technique scheme, high-temperature roasting can destroy the crystalline structure of potassium-bearing shale, and Calcium Chloride Powder Anhydrous can be accelerated speed of response between the melting positively charged ion as fusing assistant, thereby makes insoluble potassium be activated and change soluble potassium into, more just can leach potassium ion with the leaching agent lixiviate.Gained potassium leach liquor is when the preparation nitrogen-phosphorus-potassium compound fertilizer, and in phosphoric acid and ammoniacal liquor and leach liquor, the potassium ion of free state reacts, and potassium ion is separated out so that the mode of crystal form is separated as a result.
Compared with prior art, the present invention is take Calcium Chloride Powder Anhydrous as fusing assistant, accelerated the reaction between the melting positively charged ion, whole extracting method is simple, reaction time is short, can effectively extract non-dissolubility potassium from potassium-bearing shale, the extraction yield of potassium can reach 90%, and the inventive method raw material resources reserves used are huge, gained potassium vat liquor can directly be used for preparing nitrogen-phosphorus-potassium compound fertilizer and reach composite fertilizer (GB 15063-2009) lower concentration index, and wherein the content of potassium all more than 4%, solves the problem of China's potash fertilizer shortage.
Embodiment
Embodiment 1: get potassium content and be calculated as the potassium-bearing shale of 4-6% with potassium oxide, be crushed to granularity-0.074mm, get the potassium-bearing shale 400g after pulverizing, with 600g Calcium Chloride Powder Anhydrous mixing, put into retort furnace, at 800 ℃ of lower roasting 60min, be cooled to room temperature, use 1000ml H
OLeaching agent lixiviate 60min gets the potassium leach liquor after filtration, in leach liquor, potassium is take the concentration of potassium oxide calculating as 15 g/L～20 g/L, and the extraction yield of potassium can reach 90%, leaching agent H
0That mass percentage concentration is 10% H
2O
2The aqueous solution.
Adding concentration in leach liquor is that 20% phosphoric acid and concentration are each 50ml of ammoniacal liquor of 25% again, until solution crystallization fully after, filtering drying obtains potassium content and is 3.76% nitrogen-phosphorus-potassium compound fertilizer.
Embodiment 2: get potassium content and be calculated as the potassium-bearing shale of 4-6% with potassium oxide, be crushed to granularity-0.074mm, get the potassium-bearing shale 600g after pulverizing, with 900g Calcium Chloride Powder Anhydrous mixing, put into retort furnace, at 800 ℃ of lower roasting 60min, be cooled to room temperature, use 1500mlH
OLeaching agent lixiviate 60min filters, and gets the potassium leach liquor, and in leach liquor, potassium is take the concentration of potassium oxide calculating as 15 g/L～20 g/L, and the extraction yield of potassium can reach 80%～90%, leaching agent H
0That mass percentage concentration is 5% H
2O
2The aqueous solution.
Adding concentration in leach liquor is that 25% phosphoric acid and concentration are each 50ml of ammoniacal liquor of 30% again, until solution crystallization fully after, filtering drying obtains potassium content and is 3.76% nitrogen-phosphorus-potassium compound fertilizer.
Embodiment 3: get potassium content and be calculated as the potassium-bearing shale of 4-6% with potassium oxide, be crushed to granularity-0.07mm, get the potassium-bearing shale 600g after pulverizing, with 600g Calcium Chloride Powder Anhydrous mixing, put into retort furnace, at 1000 ℃ of lower roasting 70min, be cooled to room temperature, use 1500mlH
OLeaching agent lixiviate 50min filters, and gets the potassium leach liquor.The concentration that in leach liquor, potassium calculates take potassium oxide is as 15 g/L～20 g/L, the extraction yield 80%～90% of potassium, leaching agent H
0That mass percentage concentration is 1% H
2O
2The aqueous solution.
Embodiment 4: get potassium content and be calculated as the potassium-bearing shale of 4-6% with potassium oxide, be crushed to granularity-0.08mm, get the potassium-bearing shale 400g after pulverizing, with 800g Calcium Chloride Powder Anhydrous mixing, put into retort furnace, at 600 ℃ of lower roasting 50min, be cooled to room temperature, use 1000mlH
OLeaching agent lixiviate 70min filters, and gets the potassium leach liquor.In leach liquor, potassium is take the concentration of potassium oxide calculating as 15 g/L～20 g/L, and the extraction yield of potassium can reach 80%～90%, leaching agent H
0That mass percentage concentration is 8% H
2O
2The aqueous solution.
Claims (7)
1. a method of extracting potassium from potassium-bearing shale, is characterized in that: get potassium-bearing shale, pulverize rear and Calcium Chloride Powder Anhydrous mixing, 600-1000 ℃ of lower roasting, be cooled to room temperature, use leaching agent H
0Leach, after filtering, filtrate is the potassium leach liquor, wherein leaching agent H
0That mass percentage concentration is the H of 1-10%
2O
2The aqueous solution.
2. according to the described method of extracting potassium from potassium-bearing shale of claim 1, it is characterized in that: get potassium-bearing shale, pulverize rear and Calcium Chloride Powder Anhydrous mixing, at 700-900 ℃ of lower roasting 50-70min, be cooled to room temperature, use leaching agent H
0Lixiviate 50-70min filters, and filtrate is the potassium leach liquor, wherein leaching agent H
0That mass percentage concentration is the H of 4-8%
2O
2The aqueous solution.
3. according to the described method of extracting potassium from potassium-bearing shale of claim 1 or 2, it is characterized in that: potassium-bearing shale is crushed to granularity is-0.07～-0.08mm.
4. according to the described method of extracting potassium from potassium-bearing shale of claim 3, it is characterized in that: potassium-bearing shale is divided be crushed to granularity and be-0.074mm.
5. according to the described method of extracting potassium from potassium-bearing shale of claim 1 or 2, it is characterized in that: the weight ratio of potassium-bearing shale and Calcium Chloride Powder Anhydrous is 1:1-2.
6. according to the described method of extracting potassium from potassium-bearing shale of claim 5, it is characterized in that: the weight ratio of potassium-bearing shale and Calcium Chloride Powder Anhydrous is 1:1.5.
7. according to the described method of extracting potassium from potassium-bearing shale of claim 1 or 2, it is characterized in that: add phosphoric acid and ammoniacal liquor in the potassium leach liquor, the fully rear filtering drying of solution crystallization had both got nitrogen-phosphorus-potassium compound fertilizer.
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|---|---|---|---|
| CN2011104379263A CN103172410A (en) | 2011-12-23 | 2011-12-23 | Method for extracting potassium from potassium-containing shale |
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| CN2011104379263A CN103172410A (en) | 2011-12-23 | 2011-12-23 | Method for extracting potassium from potassium-containing shale |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355813A (en) * | 2014-10-29 | 2015-02-18 | 贵州省化工研究院 | Method for producing organic-inorganic compound fertilizer through potassium-bearing shale |
| CN105177312A (en) * | 2015-08-04 | 2015-12-23 | 铜仁学院 | Method for extracting potassium from shale containing potassium |
| 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 |
| CN106810320A (en) * | 2017-01-17 | 2017-06-09 | 华南农业大学 | Application and manufacture method of the activator in terms of cooling calcining manufacture activation potash fertilizer |
| CN112758937A (en) * | 2021-01-14 | 2021-05-07 | 襄阳泽东化工集团有限公司 | Method for preparing potassium fluosilicate and NPK compound fertilizer from phosphorus-potassium associated ore |
| CN113173584A (en) * | 2021-04-21 | 2021-07-27 | 武汉工程大学 | Resource comprehensive utilization method of phosphorus tailings and potassium feldspar |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355813A (en) * | 2014-10-29 | 2015-02-18 | 贵州省化工研究院 | Method for producing organic-inorganic compound fertilizer through potassium-bearing shale |
| CN105177312A (en) * | 2015-08-04 | 2015-12-23 | 铜仁学院 | Method for extracting potassium from shale containing potassium |
| 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 |
| CN106219578B (en) * | 2016-07-22 | 2018-01-09 | 中国科学院青海盐湖研究所 | A kind of preparation method of water-soluble sylvite |
| CN106810320A (en) * | 2017-01-17 | 2017-06-09 | 华南农业大学 | Application and manufacture method of the activator in terms of cooling calcining manufacture activation potash fertilizer |
| CN112758937A (en) * | 2021-01-14 | 2021-05-07 | 襄阳泽东化工集团有限公司 | Method for preparing potassium fluosilicate and NPK compound fertilizer from phosphorus-potassium associated ore |
| CN113173584A (en) * | 2021-04-21 | 2021-07-27 | 武汉工程大学 | Resource comprehensive utilization method of phosphorus tailings and potassium feldspar |
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Application publication date: 20130626 |