CN103787696B - A kind of preparation method containing potassic fertilizer and containing K composite fertilizer - Google Patents
A kind of preparation method containing potassic fertilizer and containing K composite fertilizer Download PDFInfo
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- CN103787696B CN103787696B CN201410056394.2A CN201410056394A CN103787696B CN 103787696 B CN103787696 B CN 103787696B CN 201410056394 A CN201410056394 A CN 201410056394A CN 103787696 B CN103787696 B CN 103787696B
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Abstract
The invention discloses a kind of preparation method containing potassic fertilizer, comprising: (1) sylvite ore obtains ore particles through broken, grinding; In described sylvite ore, silt content is 20 ~ 40wt%, and KCE content is 10 ~ 19wt%; (2) ore particles and solvent are mixed with the slip that mass concentration is 25 ~ 40%, obtain rich mud overflow through desliming; (3) rich mud overflow obtains rough concentrate through flotation, and this rough concentrate is for containing potassic fertilizer.The invention also discloses containing this containing the compound manure of potassic fertilizer.The present invention revolves the overflow of desliming for raw material with water, utilize flotation process flotation Repone K, add other fertilizer, as nitrogenous fertilizer, phosphate fertilizer, make composite fertilizer, like this, improve the yield of overall Repone K, also improve resource utilization, both reduce the production cost of composite fertilizer, higher than the fertility of the composite fertilizer of same content again, also improve comprehensive resource utilization rate.
Description
Technical field
The invention belongs to Salt Lake Chemistry field, be specifically related to a kind of preparation method containing potassic fertilizer and contain K composite fertilizer.
Background technology
World's potassium resource is very abundant, and the overwhelming majority is solid potassium salt ore deposit, underground, and small part is for containing potassium bittern, and resource distribution mainly concentrates on Canada, Russia, Byelorussia and Germany, and four countries' sylvite reserves account for 93% of world's total amount.Potash Resources in China is deficient, mainly based on salt lake type sylvite ore, integrated distribution in Qinghai, Xinjiang, the provinces and regions such as Tibet, explored potassium resource is mainly distributed in the Cha Er Han of Chaidamu Basin, Qinghai Province and the Lop Nur in Xinjiang; And salt lake type sylvite deposit solid potassium salt is few, and there is technical difficulty in its exploitation.
The brave wild well sylvite ore of Yunnan Province's Simao Diqu, compared with being rich in sylvite ore resource, has the features such as the low and dopant species of KCE content is many with the world.It can be divided into the sylvite ore of two types from outward appearance: one is Steel Gray sylvite ore, KCE content 13% ~ 19%, and water-insoluble, generally below 5%, reaches 10% individually; Another kind is greyish-green sylvite ore, KCE content 10% ~ 16%, and water-insoluble, generally about 30% ~ 40%, reaches 45% individually, containing a large amount of clay components, particularly complex structure in the water-insoluble in this ore deposit, brings very large difficulty to mining and processing.
Up to now, report more rarely seen to the research that height contains mud, the processing technology of low grade potassium salt mine is correlated with and industrialization.Greyish-green sylvite ore argillaceous class water-insoluble amount is high, must could for the production of potash fertilizer by removing thin mud, and the desliming of greyish-green sylvite ore is a gordian technique.Adopt simple conventional hydrocyclone machinery Desliming method, in gained concentrate water-insoluble total content, thin pureed insolubles content accounts for about 55% of total amount, and superfine mud and mother liquor are mixed into one, extremely difficult separation.Greyish-green sylvite contains a large amount of water-insolubles, dissociate at ore grinding and flotation operation process and obtain very thin pureed dispersion, these pureed dispersions have very strong activity, can adsorb the collecting agent of sylvite, become the inhibitor of sylvite, reduce the flotation yield of sylvite.Although at the thin mud of part that desliming process can remove, in flotation operation, through repeatedly high strength scouring, the thin mud being contained in salt and coarse-grained material can be dissociated out again and cause detrimentally affect to flotation.In desliming process and floatation process, the mother liquor in slip contains the water-insoluble of ultrafine particle level, and lumping together with mother liquor is difficult to be separated, and causes the accumulation of impurity in circulating mother liquor, causes great difficulty to sylvite processing.
Disclose a kind of high working method containing mud sylvite ore in patent documentation CN102976364A, by carrying out high-temperature roasting to height containing mud sylvite ore, changing physics, the chemical property of mud boulder matter, and then carrying out the extraction Repone K of flotation.Hu Xiuyuan describes Shanghai Chemical Engineering Design Inst. and adopts dissolving crystallized method to some research work of Yunnan sylvite ore.Xu Qintang adopts water soluble method adopts halogen, thermo-compression evaporation salt manufacturing and vacuum cold crystallization technology reclaim Repone K technical process to carry out the exploitation in Jiang Cheng sylvite mineral deposit, Yunnan.Aforesaid method all exists that Technology complexity, energy consumption are large, high in cost of production defect, thus causes it industrially cannot apply.
Method main study subject disclosed in Chinese patent literature CN102008999B, CN101982412B, CN103145152A is higher-grade Repone K (35% ~ 50%), the processing of (2% ~ 8%) sylvite ore that water insoluble matter content is low, and the greyish-green sylvite ore of the brave wild well in city, Yunnan Province of China river belongs to low-grade (KCl≤13%), high clay (water-insoluble >=30%) sylvite ore.For many years, adopt rich ore and abandon lean ore, make in existing mining well, to have accumulated a large amount of greyish-green lean ores, have a strong impact on the survival and development of normally carrying out of producing and enterprise.By geologic report total reserves, greyish-green sylvite ore accounts for about 60%, and uses existing technology cannot to process these sylvite ore, causes the waste of resource.And corresponding, China is restricted in potash fertilizer throughput always.
The basic skills of current domestic production composite fertilizer is: buy Repone K finished product, then adds nitrogenous fertilizer and phosphate fertilizer, separately adds some fillers again, and it exists the problem that the high and starting material of product cost need to purchase respectively transport.
Summary of the invention
The object of the invention is to overcome the problem that in prior art, potash fertilizer production cost is high, provide a kind of and produced the method containing K composite fertilizer by poor sylvite ore.
Described method comprises:
(1) sylvite ore obtains ore particles through broken, grinding.In described sylvite ore, silt content is 20 ~ 40wt%, and KCE content is 10 ~ 19wt%.
Described ore can be the composite ore of greyish-green sylvite raw ore or itself and Steel Gray sylvite ore, or any other contains the ore composition of Repone K and mud, and it all goes for method of the present invention.
Preferably, sylvite ore is crushed to the ore particles being less than 40mm by described fragmentation, and then grinds.
Those skilled in the art can select the granularity of broken rear ore particles as required voluntarily, such as ore salt mine are crushed to 30mm, and then are ground to 1 ~ 2mm, and set corresponding fragmentation and abrasive parameters according to the globule size for grinding.Preferably, select 2mm as the particle diameter of final ore particles, although too small particle diameter is conducive to follow-up process, the lifting of cost can be brought undoubtedly; Excessive particle diameter is then unfavorable for the extraction of Repone K in subsequent process.
Preferably, described in be ground to ball milling or rod milling, milling liquid medium is the common saturated solution of Repone K and sodium-chlor.During ball milling, sylvite ore after fragmentation enters rod mill or ball mill through pendulum feeder, weighing belt, add the common saturated solution of Repone K and the sodium-chlor certainly flow down from header tank at mill entrance place simultaneously, grinding machine outlet ore pulp revolves through water the particle filter that grading machine or screw classifier carry out mineral, the mineral grain making Task-size Controlling be less than certain limit enters next technical process, and granularity be greater than this scope mineral return rod mill or ball mill, proceed grinding.
(2) ore particles and solvent are mixed with the slip that mass concentration is 25 ~ 40%, obtain rich mud overflow through desliming.
Preferably, described desliming comprises the hydrocyclone desliming being no less than twice, hydrocyclone desliming each time all obtains corresponding overflow and underflow, and wherein overflow is used for hydrocyclone desliming next time, and described rich mud overflow is the overflow that the desliming of final stage hydrocyclone obtains.The component that hydrocyclone obtains has included most insolubles and the fertilizer containing potassium, extra repeatedly current eddy flow desliming is carried out for a hydrocyclone, and collect its corresponding overflow, can enrichment water-insoluble, and remove unnecessary salt component as much as possible.
Preferred, described desliming comprises twice hydrocyclone desliming, and it is rich mud overflow that the overflow of a described desliming obtains overflow after secondary desliming.
When carrying out hydrocyclone process, inevitably, in a hydrocyclone, carried part insolubles secretly, these insolubless for Repone K preparation be harmful, but for preparation containing for potassic fertilizer, it brings again unnecessary loss.Therefore, be necessary to recycle these insolubless, optional scheme carries out hydrocyclone desliming again to the underflow that hydrocyclone obtains, and the overflow obtained is reclaimed.Preferably, described desliming comprises the hydrocyclone desliming being no less than two-stage, every grade of hydrocyclone desliming all obtains overflow and underflow, described underflow enters subordinate's hydrocyclone desliming, the overflow obtained is back to the desliming of first step hydrocyclone or the desliming of upper level current eddy flow, and it also obtains corresponding overflow and underflow; The hydrocyclone desliming of the overflow that the desliming of described first step hydrocyclone obtains more than once obtains rich mud overflow.Adopt twice hydrocyclone, that can effectively avoid insolubles to utilize for underflow bothers, and avoids the loss of insolubles; Herein, owing to having carried out one-level hydrocyclone desliming process, follow-uply only need to carry out once above hydrocyclone desliming and namely can obtain rich mud overflow.
As preferred technical scheme, described desliming comprises the desliming of two-stage hydrocyclone, described slip enters and obtains one-level overflow and one-level underflow through the desliming of one-level hydrocyclone, described one-level underflow obtains secondary underflow and secondary overflow through the desliming of secondary hydrocyclone, and described secondary overflow returns carries out desliming through one-level current eddy flow; Described one-level overflow obtains rich mud overflow through the desliming of secondary hydrocyclone.
Preferably, described desliming comprises the hydrocyclone desliming of one-level, and described rich mud overflow is the overflow of hydrocyclone desliming.
Preferably, described solvent is the common saturated mother liquor of Repone K and sodium-chlor.
Preferably, described desliming comprises the desliming of two-stage hydrocyclone.
(3) rich mud overflow obtains rough concentrate through flotation.Not only containing Repone K fertilizer in described rough concentrate, and owing to wherein having sandwiched a certain amount of water-insoluble, these water-insolubles contain a certain amount of organic rotten machine matter, they are alternative a certain amount of filler both, there is again certain fertility, can provide the fertilizer efficiency of fertilizer, itself namely can as Fertilizer application; But at present, not yet there is this rough concentrate of report can be used as containing potassic fertilizer.In this rough concentrate, the content of Repone K is 45 ~ 55%, and the content of sodium-chlor is 15 ~ 20%, and the content of the molten thing in water portion is 25 ~ 40%.
Preferably, the medicament used during flotation is 18 amine, and its consumption is 300 ~ 400g/ raw material, and during flotation, stirring velocity is 1700 ~ 1800r/min, flotation time 8 ~ 10min.
Present invention also offers a kind of include above-mentioned rough concentrate containing K composite fertilizer.Containing in K composite fertilizer, the addition of other elements can add according to the standard of country or actual needs, this can select as required and flexibly for those skilled in the art, such as during outstanding phosphorus content, first can measure the content of phosphorus in rough concentrate, add phosphorous fertilizer and other batchings afterwards, such as nitrogenous raw material.
The present invention revolves the overflow of desliming for raw material with water, utilize flotation process flotation Repone K, add other fertilizer, as nitrogenous fertilizer, phosphate fertilizer, make composite fertilizer, like this, improve the yield of overall Repone K, also improve resource utilization, both reduce the production cost of composite fertilizer, higher than the fertility of the composite fertilizer of same content again, also improve comprehensive resource utilization rate.
Accompanying drawing explanation
Fig. 1, twice water revolve the schematic flow sheet of legal system for rich mud overflow.
Fig. 2, a water revolve the schematic flow sheet of legal system for rich mud overflow.
Fig. 3, two-stage water revolve the schematic flow sheet of legal system for rich mud overflow.
Embodiment
Be below a preferred embodiment of the application, it is only used as the explanation of the application instead of restriction.
As Fig. 1 ~ 3, the invention provides the method for the rich mud overflow of multiple preparation, in the present embodiment, the overflow slip of experiment, it obtains as follows:
See Fig. 1: greyish-green sylvite or mixed potassium halite raw material, through broken, ore grinding to 0.5 ~ 1.0mm, hydrocyclone is utilized to carry out secondary desliming, hydrocyclone desliming once all obtains primary overflow and a underflow, wherein primary overflow is used for the desliming of secondary hydrocyclone, and described rich mud overflow is the overflow that the desliming of secondary hydrocyclone obtains.
See Fig. 2: greyish-green sylvite or mixed potassium halite raw material, through broken, ore grinding to 0.5 ~ 1.0mm, utilize hydrocyclone to carry out secondary desliming, the overflow that hydrocyclone desliming once all obtains is rich mud overflow.
See Fig. 3: greyish-green sylvite or mixed potassium halite raw material, through broken, ore grinding to 0.5 ~ 1.0mm, hydrocyclone is utilized to carry out secondary desliming, the hydrocyclone desliming of one-level all obtains one-level overflow and one-level underflow, wherein one-level overflow is used for the desliming of secondary hydrocyclone, and described rich mud overflow is the overflow that the desliming of secondary hydrocyclone obtains; One time underflow is concentrate through the underflow that the desliming of secondary hydrocyclone obtains, direct flotation preparing potassium chloride, and overflow returns continuation desliming.
Employ rich mud overflow prepared by Fig. 1 and Fig. 3 method below in an example through subsequent disposal as containing potassic fertilizer, for containing the larger raw material of insolubles content, also the method shown in Fig. 2 can be taked to prepare rich mud overflow, and it also can play similar technique effect.
Its composition of the raw material that embodiment 1 ~ 3 adopts is as table 1.
Table 1. experimental raw compositional analysis result
| KCl/% | NaCl/% | WI/% | H 2O/% | Concentration/% |
| 9.83 | 27.98 | 60.97 | 30.91 | 8.0 |
The concrete technology step utilizing overflow slip to obtain Repone K rough concentrate and composite fertilizer is:
(1) raw material is extracted: get secondary water and revolve that desliming overflow raw material is some to stir, for flotation experiments.
(2) flotation test: get raw material slip 1800mL, joins XFD III type unit flotation cell; Experiment condition: stirring velocity 1800r/min, 18 amine consumptions are 400g/t raw material, and flotation time 10min, roughly selects through one-level, can obtain Repone K rough concentrate.
(3) rougher concentration after filtration, can obtain Potassium Chloride Product.Experimental result is in table 2.
(4) this product drying, is the thick product of Repone K, can mixes according to a certain percentage, make composite fertilizer with nitrogen phosphorus fertilizer.
Embodiment 1: raw material revolves desliming overflow for method shown in Fig. 3 obtains secondary water.Get raw material 1800ml, join XFD III type unit flotation cell, flotation conditions: mixing speed is 1700r/min; The pharmacy effect time is 5min; Flotation time is 8min; 18 amine add-ons are 300g/ ton raw material.Experimental result is in table 2.This concentrate can be configured to composite fertilizer after drying by a certain percentage, and its composition is as shown in table 2.
Table 2: experimental result
Embodiment 2: raw material revolves desliming overflow for the secondary of method shown in Fig. 1 water.Get raw material 1800ml, join XFD III type unit flotation cell, flotation conditions: mixing speed: 1800r/min; The pharmacy effect time: 5min; Flotation time: 10min; 18 amine add-ons: 400g/ ton raw material.Experimental result is in table 3.This concentrate can be configured to composite fertilizer after drying by a certain percentage, and its composition is as shown in table 3.
Table 3: experimental result
Embodiment 3: raw material is that Fig. 1 secondary water revolves desliming overflow.Get raw material 1800ml, join XFD III type unit flotation cell, flotation conditions: mixing speed: 1800r/min; The pharmacy effect time: 5min; Flotation time: 10min; 18 amine add-ons: 400g/ ton raw material.Experimental result is in table 4.This concentrate can be configured to composite fertilizer after drying by a certain percentage, and its composition is as shown in table 4.
Table 4: experimental result
In above-mentioned table, γ is productive rate; ε is yield, and its method of calculation are: using the yield of the Repone K sum of concentrate and tailings as the total of Repone K.
Claims (8)
1., containing a preparation method for potassic fertilizer, comprising:
(1) sylvite ore obtains ore particles through broken, grinding; In described sylvite ore, silt content is 20 ~ 40wt%, and KCE content is 10 ~ 19wt%;
(2) ore particles and solvent are mixed with the slip that mass concentration is 25 ~ 40%, obtain rich mud overflow through desliming; Described desliming comprises the hydrocyclone desliming being no less than twice, and hydrocyclone desliming each time all obtains overflow and underflow, and wherein overflow is used for hydrocyclone desliming next time, and described rich mud overflow is the overflow that the desliming of last hydrocyclone obtains; Described solvent is the common saturated mother liquor of Repone K and sodium-chlor;
(3) rich mud overflow obtains rough concentrate through flotation, and this rough concentrate is for containing potassic fertilizer.
2. method according to claim 1, is characterized in that, described desliming comprises twice hydrocyclone desliming, and it is rich mud overflow that the overflow of a described desliming obtains overflow after secondary desliming.
3. method according to claim 1, it is characterized in that, described desliming comprises the hydrocyclone desliming being no less than two-stage, every grade of hydrocyclone desliming all obtains overflow and underflow, the underflow obtained enters subordinate's hydrocyclone desliming, and the overflow obtained is back to the desliming of first step hydrocyclone or the desliming of upper level current eddy flow; The overflow that the hydrocyclone desliming of the overflow that the desliming of first step hydrocyclone obtains more than once obtains is rich mud overflow.
4. method according to claim 3, it is characterized in that, described desliming comprises the desliming of two-stage hydrocyclone, described slip enters and obtains one-level overflow and one-level underflow through the desliming of one-level hydrocyclone, described one-level underflow obtains secondary underflow and secondary overflow through the desliming of secondary hydrocyclone, and described secondary overflow returns carries out desliming through one-level current eddy flow; Described one-level overflow is rich mud overflow through the overflow that the desliming of secondary hydrocyclone obtains.
5. method according to claim 1, is characterized in that, described desliming comprises the hydrocyclone desliming of one-level, and described rich mud overflow is the overflow of hydrocyclone desliming.
6. method according to claim 1, is characterized in that, the medicament that described flotation uses is 18 amine, and its consumption is 300 ~ 400g/ raw material, and during flotation, stirring velocity is 1700 ~ 1800r/min, flotation time 8 ~ 10min.
7. what claim 1 ~ 6 either method prepared contains potassic fertilizer.
8. containing containing potassic fertilizer described in claim 7 containing K composite fertilizer.
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| CN104163440A (en) * | 2014-08-27 | 2014-11-26 | 中国科学院青海盐湖研究所 | Method for producing KCl from ground surface carnallite |
| CN106311455A (en) * | 2016-08-25 | 2017-01-11 | 湖南顺源陶瓷材料有限公司 | Desliming process for nonmetal mineral separation |
Citations (5)
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| SU1527230A1 (en) * | 1987-08-11 | 1989-12-07 | Белорусский филиал Всесоюзного научно-исследовательского и проектного института галургии | Method of producing potassium chloride |
| CN1259486A (en) * | 1999-01-04 | 2000-07-12 | 化学工业部连云港设计研究院 | Method of extracting potassium chloride from mixed ore of sylvine and carnallite |
| CN101982412A (en) * | 2010-11-09 | 2011-03-02 | 化工部长沙设计研究院 | Process for extracting KCl coarse grains by carrying out flotation on solid sylvinite primary ores |
| CN102198429A (en) * | 2011-02-22 | 2011-09-28 | 化工部长沙设计研究院 | Flotation desliming process for solid sylvite mineral containing slime |
| CN103145152A (en) * | 2013-04-11 | 2013-06-12 | 中蓝连海设计研究院 | Process for extracting potassium chloride by coarse flotation of primary sylvine ores |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1527230A1 (en) * | 1987-08-11 | 1989-12-07 | Белорусский филиал Всесоюзного научно-исследовательского и проектного института галургии | Method of producing potassium chloride |
| CN1259486A (en) * | 1999-01-04 | 2000-07-12 | 化学工业部连云港设计研究院 | Method of extracting potassium chloride from mixed ore of sylvine and carnallite |
| CN101982412A (en) * | 2010-11-09 | 2011-03-02 | 化工部长沙设计研究院 | Process for extracting KCl coarse grains by carrying out flotation on solid sylvinite primary ores |
| CN102198429A (en) * | 2011-02-22 | 2011-09-28 | 化工部长沙设计研究院 | Flotation desliming process for solid sylvite mineral containing slime |
| CN103145152A (en) * | 2013-04-11 | 2013-06-12 | 中蓝连海设计研究院 | Process for extracting potassium chloride by coarse flotation of primary sylvine ores |
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