CN104891533A - Method for preparing potassium sulphate by virtue of potassium-enriched slate and desulfurization gypsum - Google Patents
Method for preparing potassium sulphate by virtue of potassium-enriched slate and desulfurization gypsum Download PDFInfo
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- CN104891533A CN104891533A CN201510276458.4A CN201510276458A CN104891533A CN 104891533 A CN104891533 A CN 104891533A CN 201510276458 A CN201510276458 A CN 201510276458A CN 104891533 A CN104891533 A CN 104891533A
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- potassium sulfate
- desulfurated plaster
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Abstract
The invention relates to a method for preparing potassium sulphate by virtue of potassium-enriched slate and desulfurization gypsum, relates to the field of environment protection, and belongs to a solid waste treatment technology. The method comprises the following steps: proportioning potassium-enriched slate, desulfurization gypsum, calcium carbonate and pulverized coal in a certain ratio and crushing the raw materials to a certain extent, then adding a small amount of running water to carry out wet mixing, pressing the mixture into blocks after the mixing is complete, and conveying the pressed samples to a roasting procedure; roasting for a certain time at a specified temperature and then taking out the samples, cooling the samples to room temperature in air to obtain a roasted product containing potassium sulphate, crushing the roasted product and then conveying the roasted product to a leaching procedure; leaching under a certain liquid-solid ratio, filtering, collecting the filtrate, precipitating and removing impurities, and collecting a clear solution; and evaporating and concentrating the clear solution, and cooling and crystallizing to obtain potassium sulphate. According to the method disclosed by the invention, the high-potassium characteristic of the potassium-enriched slate is adequately utilized, and the steel-cladding desulfurization gypsum is reasonably utilized, thus the current situation of short potassium resources of China can be made up to a certain extent, and the pollution of desulfurization gypsum accumulation to environment is avoided simultaneously.
Description
Technical field
The present invention relates to a kind of method that Bayan Obo k-rich slate thermolysis generates potassium sulfate, relate to field of Environment Protection, belong to solid waste resource recovery treatment technology.
Background technology
China is a large agricultural country, and the population exceeding the world 20% is supported in the soil with plough less than the world 1/10th, and China must improve constantly grain yield for this reason, and potash fertilizer is most important as the growth of the requisite fertilizer of farm crop to farm crop.But the potash fertilizer of China consumption breach is comparatively large, the degree of self-sufficiency only has 58%, needs a large amount of imports.The dependence on external supply undue to potash fertilizer, this threatens the grain security of China, and therefore, the self-produced potash fertilizer output improving country is the task of top priority.
At present, the main raw material that China produces potash fertilizer is salt lake brine, and these salt lake brines are mainly distributed in western Qinghai, Xinjiang Lop Nur etc. and have inconvenient traffic, and the area that Infrastructure falls behind limits the throughput of enterprise, more can not meet domestic needs.Therefore, fully developing on the basis of salt lake resources and seawater Potash Resources, water-insoluble potassium resource must developed further, improve domestic self-produced potassium output, for China's agriculture production provides safety control.
Packet header Baiyunebo iron mine be one based on the oversized mineral deposit of iron, rare earth, niobium, wherein dolomite stratigraph and slate layer distributed more widely, and the elements such as iron, niobium, rare earth, potassium mainly compose be stored in this two-layer among.K-rich slate is mainly composed and is stored among slate layer, is distributed in iron ore body and coils, its reserves more than 1.67 hundred million tons, average K
2o content is more than 11%.Along with a large amount of exploitations of Baiyunebo iron mine, the k-rich slate that annual exploitation is peeled off is more than 2,000,000 tons, and the k-rich slate that these are stripped also is in the stacking stage without disposing at present substantially, takies a large amount of soil.
The potassium-bearing mineral of potassium rich rock is mainly potassium felspar sand, crystal-chemical formula KAlSi
3o
8, theory consists of (massfraction): SiO
2%=64.7%, Al
2o
3%=18.4%, K
2o%=16.9%.Potassium felspar sand is a kind of non-water-soluble sylvite, its stable chemical nature, Al, Si, O be wherein with stable tetrahedron reticulated structure exist, at normal temperatures and pressures except hydrofluoric acid be difficult to dissolve by other soda acids.The method that k-rich slate extracts sylvite has a lot, still there is material impact so far or mainly contain four kinds in lasting research, one is potassium felspar sand-sodium carbonate intermediate sintering temperature method, but the higher and large usage quantity of sodium carbonate price, its follow-up technical process control accuracy requirement is higher; The second is potassium felspar sand-sodium hydroxide hydrothermal method, but the amount that this reaction consumes NaOH is comparatively large, and at this temperature, the requirement of existence to reactor of highly basic is higher, and potassium felspar sand utilization ratio is lower, is difficult to industrial applications; The third is potassium felspar sand-sulfuric acid-phosphorite low-temperature pickling process, but reaction intermediate HF etc. propose safely certain requirement to conversion unit and production operation, and reaction also creates a large amount of lime feldspar and quartzy tailings simultaneously; 4th kind is potassium felspar sand-calcium sulfate-calcium carbonate high-temperature roasting method; document 1(institution of higher education Journal of Chemical Industry and Engineering; 1998; 19 (3): 347) report; prepare burden by m (potassium felspar sand): m (gypsum): m (calcium carbonate)=1:1:3; roasting 3.0h under 1323K, the rate of decomposition of potassium can reach 83.4%, and the main Problems existing of the method is that calcium carbonate usage quantity causes greatly tailings quantity discharged large.
Therefore, a kind of cost of urgent need exploitation is low, material consumption is little, the k-rich slate of raw material availability advantages of higher puies forward potassium technology.
Summary of the invention
The object of the present invention is to provide a kind of method of k-rich slate and desulfurated plaster thermolysis preparing potassium sulfate, to realize the efficiency utilization to k-rich slate, process a part of desulfurated plaster simultaneously, alleviate the present situation of China's potassium resource shortage, realize the comprehensive utilization of resources of solid waste.
Technical scheme of the present invention is: adopt k-rich slate-desulfurated plaster-calcium carbonate-coal dust concurrent roasting thermal decomposition method to prepare potassium sulfate, the method specifically comprises the following steps:
Step (1) ball milling operation:
K-rich slate, desulfurated plaster, calcium carbonate are pulverized by after proportion ingredient, was ground to 100 mesh sieves, for subsequent use;
Step (2) wet mixing operation:
The tap water being added 0.05% ~ 0.10% (massfraction) in the mixture that step (1) is obtained carries out wet mixing, fully stirs, mixing;
Step (3) briquetting operation:
The described mixture obtained toward step (2) carries out briquetting under 2MPa ~ 10MPa pressure, obtains sample, for subsequent use;
Step (4) calcining process:
Described sample step (3) obtained, at a certain temperature after roasting certain hour, obtains calcining matter and is sent to pulverizing process;
Step (5) pulverizing process:
The described calcining matter that step (4) obtains is fed in sample grinding machine and carries out being crushed to 80 mesh sieves, obtain the powder of sulfur acid potassium, for subsequent use;
Step (6) leaches operation:
Described sulfur acid potassium potassium powder step (5) obtained and tap water carry out mix and blend leaching with certain proportion, and extraction time is 0.5 ~ 2 hour, obtains mixed solution, for subsequent use;
Step (7) filter progress:
Described mixed solution step (6) obtained is sent into filter progress and is filtered, and will obtain leached mud and leach liquor, and the described leached mud obtained is used as cement-based material, and the described leach liquor obtained is sent to removal of impurities operation;
Step (8) removing impurity by means of precipitation operation:
Described leach liquor step (7) obtained adds precipitation agent with the amount of 0.5 ~ 2g/L and carries out removing impurity by means of precipitation in removal of impurities operation, and after precipitation is complete, stratification or filtration, collect clear liquid;
Step (9) evaporative crystallization operation:
The described clear liquid that step (8) obtains is entered evaporative crystallization operation, carries out negative pressure evaporation crystallization operation to clear liquid, evaporation concentration is to 2/5 ~ 3/5 of original volume, and crystallisation by cooling, obtains crystallisate potassium sulfate after centrifugation; Wherein crystalline mother solution returns the leaching operation of step (6).
K-rich slate described in described step (1), desulfurated plaster, calcium carbonate are 1:(0.5 ~ 1 with addition of mass ratio): (1.5 ~ 2.5), also can add coal dust, the addition of described coal dust is 3% ~ 7%(massfraction).
Described in described step (4), maturing temperature is 1323K ~ 1423K, and roasting time is 30min ~ 60min.
The blending ratio containing potassium powder and tap water described in described step (6) is 1:2 ~ 1:5 (g/ml).
Described in described step (7), precipitation agent is potassium sulfate or salt of wormwood.
Compared with the present invention produces soluble potassium salt technology with existing k-rich slate, its advantage is:
(1) in the present invention, k-rich slate ore deposit roasting time is short, and the low rate of decomposition of maturing temperature is fast, and rate of decomposition high (>90%), is conducive to energy-saving and emission-reduction.
(2) the present invention is using desulfurated plaster as precipitation additive, works in coordination with preparing potassium sulfate with k-rich slate, greatly reduces raw materials cost, has both avoided the environmental pollution that desulfurated plaster causes, and achieves again solid waste resource recovery comprehensive utilization.
(3) present device is simple and easy, technical process is short, has investment low, simple to operate, economical and practical feature.
The present invention makes full use of the high potassium characteristic in k-rich slate, Appropriate application Baogang desulfurated plaster, turn waste into wealth, the present situation of China's potassium resource shortage can be made up to a certain extent, supplying raw materials for producing potash fertilizer, avoiding k-rich slate simultaneously, desulfurated plaster accumulation takies a large amount of soil and the pollution to environment.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the thermolysis of Bayan Obo k-rich slate generates potassium sulfate.
Embodiment
Embodiment 1
See Fig. 1, the method for Bayan Obo thermolysis preparing potassium sulfate of the present invention, operates as follows:
I) be 1:0.5:1.5 batching by k-rich slate, desulfurated plaster, calcium carbonate mass ratio, add the coal dust of 3% simultaneously, and raw material ball was milled to 100 mesh sieves.Then the mixture of ball milling operation is sent to wet mixing operation, the tap water adding 0.05% carries out wet mixing.
II) in briquetting operation, under the pressure of 2MPa, sample is pressed into block, the sample pressed is sent to calcining process, roasting 30min under 1323K, reaction conversion ratio is 85.45%.
III), after reaching roasting time, take out sample and be sent to pulverizing and attack speed and be coldly crushed to 80 mesh sieves.Then the potassium powder that contains after pulverizing is sent to leaching operation, mixes containing the ratio of potassium powder with tap water 1:2, agitation leach 0.5 hour.
IV) after reaching the agitation leach time, mixed solution is sent into filter progress and filters, leached mud is used as cement-based material, and removing impurity by means of precipitation operation sent into by leach liquor.
V), after leach liquor enters removing impurity by means of precipitation operation, add salt of wormwood with the amount of 0.5g/L and carry out removing impurity by means of precipitation, the time is half an hour, then stratification, collects clear liquid.
VI) supernatant liquid of removing impurity by means of precipitation operation is sent into evaporative crystallization operation, clear liquid is after evaporating 2/5 volume, and crystallisation by cooling obtains potassium sulfate (90.7%), and mother liquor returns and merges as initial leach liquor with tap water.
Embodiment 2
See Fig. 1, the method for Bayan Obo thermolysis preparing potassium sulfate of the present invention, operates as follows:
I) be 1:1:2.5 batching by k-rich slate, desulfurated plaster, calcium carbonate mass ratio, add the coal dust of 7% simultaneously, and raw material ball was milled to 100 mesh sieves.Then the mixture of ball milling operation is sent to wet mixing operation, the tap water adding 0.10% carries out wet mixing.
II) in briquetting operation, under the pressure of 10MPa, sample is pressed into block, the sample pressed is sent to calcining process, roasting 60min under 1423K, reaction conversion ratio is 96.77%.
III), after reaching roasting time, take out sample and be sent to pulverizing and attack speed and be coldly crushed to 80 mesh sieves.Then the potassium powder that contains after pulverizing is sent to leaching operation, mixes containing the ratio of potassium powder with tap water 1:5, agitation leach 2 hours.
IV) after reaching the agitation leach time, mixed solution is sent into filter progress and filters, leached mud is used as cement-based material, and removing impurity by means of precipitation operation sent into by leach liquor.
V), after leach liquor enters removing impurity by means of precipitation operation, add potassium sulfate with the amount of 2g/L and carry out removing impurity by means of precipitation, the time is half an hour, then stratification, collects clear liquid.
VI) supernatant liquid of removing impurity by means of precipitation operation is sent into evaporative crystallization operation, clear liquid is after evaporating 3/5 volume, and crystallisation by cooling obtains potassium sulfate (94%), and mother liquor returns and merges as initial leach liquor with tap water.
Embodiment 3
See Fig. 1, the method for Bayan Obo thermolysis preparing potassium sulfate of the present invention, operates as follows:
I) be 1:0.8:2 batching by k-rich slate, desulfurated plaster, calcium carbonate mass ratio, add the coal dust of 5% simultaneously, and raw material ball was milled to 100 mesh sieves.Then the mixture of ball milling operation is sent to wet mixing operation, the tap water adding 0.08% carries out wet mixing.
II) in briquetting operation, under the pressure of 8MPa, sample is pressed into block, the sample pressed is sent to calcining process, roasting 40min under 1373K, reaction conversion ratio is 93.35%.
III), after reaching roasting time, take out sample and be sent to pulverizing and attack speed and be coldly crushed to 80 mesh sieves.Then the potassium powder that contains after pulverizing is sent to leaching operation, mixes containing the ratio of potassium powder with tap water 1:3, agitation leach 1 hour.
IV) after reaching the agitation leach time, mixed solution is sent into filter progress and filters, leached mud is used as cement-based material, and removing impurity by means of precipitation operation sent into by leach liquor.
V), after leach liquor enters removing impurity by means of precipitation operation, add potassium sulfate with the amount of 1g/L and carry out removing impurity by means of precipitation, the time is half an hour, then stratification, collects clear liquid.
VI) supernatant liquid of removing impurity by means of precipitation operation is sent into evaporative crystallization operation, clear liquid is after evaporating 3/5 volume, and crystallisation by cooling obtains potassium sulfate (92%), and mother liquor returns and merges as initial leach liquor with tap water.
Claims (6)
1. utilize k-rich slate and desulfurated plaster to prepare a method for potassium sulfate, it is characterized in that, said method comprising the steps of:
Step (1) ball milling operation:
K-rich slate, desulfurated plaster and calcium carbonate are pulverized by after proportion ingredient, is ground to 100-250 mesh sieve, for subsequent use;
Step (2) wet mixing operation:
The tap water being added 0.05% ~ 0.10% (massfraction) in the mixture that step (1) is obtained carries out wet mixing, fully stirs, mixing;
Step (3) briquetting operation:
The described mixture obtained toward step (2) carries out briquetting under 2MPa ~ 10MPa pressure, obtains sample, for subsequent use;
Step (4) calcining process:
Described sample step (3) obtained is carrying out roasting, obtains calcining matter and is sent to pulverizing process;
Step (5) pulverizing process:
The described calcining matter that step (4) obtains is fed in sample grinding machine and carries out being crushed to 80-250 mesh sieve, obtain the powder of sulfur acid potassium, for subsequent use;
Step (6) leaches operation:
Powder and the tap water of described sulfur acid potassium step (5) obtained carry out mix and blend leaching, leach 0.5 ~ 2 hour, obtain mixed solution, for subsequent use;
Step (7) filter progress:
Described mixed solution step (6) obtained is sent into filter progress and is filtered, and will obtain leached mud and leach liquor, and the described leached mud obtained is used as cement-based material, and the described leach liquor obtained is sent to removal of impurities operation;
Step (8) removing impurity by means of precipitation operation:
Described leach liquor step (7) obtained adds precipitation agent with the amount of 0.5 ~ 2g/L and carries out removing impurity by means of precipitation in removal of impurities operation, and after precipitation is complete, stratification or filtration, collect clear liquid;
Step (9) evaporative crystallization operation:
The described clear liquid that step (8) obtains is entered evaporative crystallization operation, carries out evaporating, concentrating and crystallizing operation to clear liquid, evaporation concentration is to 2/5 ~ 3/5 of original volume, and crystallisation by cooling, obtains crystallisate potassium sulfate after centrifugation; Wherein crystalline mother solution returns the leaching operation of step (6).
2. according to claim 1ly utilize the thermolysis of Bayan Obo k-rich slate to generate the method for potassium sulfate, it is characterized in that: described k-rich slate, desulfurated plaster, calcium carbonate with addition of mass ratio be 1:(0.5 ~ 1): (1.5 ~ 2.5).
3. the method utilizing k-rich slate and desulfurated plaster to prepare potassium sulfate according to claim 1, is characterized in that: described step (1) is also added with coal dust, the add-on of described coal dust is massfraction 3% ~ 7%.
4. the method utilizing k-rich slate and desulfurated plaster to prepare potassium sulfate according to claim 1, is characterized in that: the maturing temperature of described step (4) is 1323K ~ 1433K, and roasting time is 30min ~ 60min.
5. the method utilizing k-rich slate and desulfurated plaster to prepare potassium sulfate according to claim 1, is characterized in that: the blending ratio of described step (6) sulfur acid potassium powder and tap water is 1:2 ~ 1:5 (g/ml).
6. the method utilizing k-rich slate and desulfurated plaster to prepare potassium sulfate according to claim 1, is characterized in that: the precipitation agent in described step (8) is potassium sulfate or salt of wormwood.
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| CN201510276458.4A CN104891533A (en) | 2015-05-26 | 2015-05-26 | Method for preparing potassium sulphate by virtue of potassium-enriched slate and desulfurization gypsum |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927881A (en) * | 2017-03-03 | 2017-07-07 | 北京科技大学 | It is a kind of to promote method of the k-rich slate thermal decomposition with roasting tailings discharge is reduced |
| CN113149037A (en) * | 2021-05-25 | 2021-07-23 | 天津渤化永利化工股份有限公司 | Method for preparing potassium sulfate by utilizing desulfurized gypsum |
| CN115849405A (en) * | 2022-12-08 | 2023-03-28 | 包头稀土研究院 | Method for co-processing potassium-rich slate and rare earth smelting white slag and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927881A (en) * | 2017-03-03 | 2017-07-07 | 北京科技大学 | It is a kind of to promote method of the k-rich slate thermal decomposition with roasting tailings discharge is reduced |
| CN113149037A (en) * | 2021-05-25 | 2021-07-23 | 天津渤化永利化工股份有限公司 | Method for preparing potassium sulfate by utilizing desulfurized gypsum |
| CN115849405A (en) * | 2022-12-08 | 2023-03-28 | 包头稀土研究院 | Method for co-processing potassium-rich slate and rare earth smelting white slag and application |
| CN115849405B (en) * | 2022-12-08 | 2024-07-26 | 包头稀土研究院 | Method for cooperatively treating potassium-rich slate and rare earth smelting white slag and application thereof |
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Application publication date: 20150909 |