CN101723408A - Method for producing potassium chloride by utilizing tertiary solid sylvite ore inverse flotation method - Google Patents
Method for producing potassium chloride by utilizing tertiary solid sylvite ore inverse flotation method Download PDFInfo
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Abstract
The invention relates to a method for producing potassium chloride by utilizing a tertiary solid sylvite ore inverse flotation method, which comprises the following steps of: firstly crushing a tertiary solid sylvite raw material ore into grains the diameter of which is smaller than 1mm, and then adding a mother liquor to obtain a slurry; then adding a floating agent into the slurry, uniformly mixing, then floating according to the flows of primary roughing, primary scavenging and primary selection and filtering to respectively obtain flotation concentrate carnallite, flotation tailing sodium chloride and a decomposition mother liquor; next, cooling the decomposition mother liquor after evaporating twice, and then totally converting the mother liquor into a magnesium chloride product; decomposing and crystallizing the flotation concentrate carnallite to obtain coarse potassium chloride; and finally repulping, washing, filtering and drying the coarse potassium chloride to obtain a potassium chloride product with the grade higher than 97 percent. In the invention, a crude ore is crushed in a simple crushing mode, and an inverse flotation process is adopted, not only effectively saving the investment and the operating cost of ore grinding equipment, but also improving the yield and the purity of the potassium chloride.
Description
Technical field
The present invention relates to a kind of method of producing Repone K, relate in particular to a kind of method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K of utilizing.
Background technology
World's potassium resource is very abundant, and total resources reaches 2,500 hundred million tons, and the overwhelming majority is underground solid sylvite, and small part mainly is distributed in North America, Europe, South America, the Middle East and countries such as Asia Thailand, Laos for containing potassium bittern.And the Potash Resources in China scarcity particularly lacks large-scale soluble solids sylvite deposit, 40 places, explored soluble potassium salt orefield, and large-scale 6 places are distributed in provinces and regions such as Qinghai, Xinjiang, Tibet, Yunnan, Shandong, Gansu.Wherein rich sylvite lake is more concentrated in the Caidamu Basin, the grade in these rich sylvite lakes is higher relatively, and its geological prospecting degree also is higher than other lake region, in addition, the exploration of sylvite is being carried out in lake region, Lop Nur, Xinjiang, and this two district can become China domestic sylvite production base.
Although country supports the potash fertilizer production of China energetically, it is newly-increased that the output doubled, but because the shortage of domestic Potash Resources, about 2,500,000 tons of the gross annual output amounts of China's potash fertilizer, and the space of expanding production is very limited, can't satisfy the huge demand of 1,000 ten thousand tons of domestic markets, at present about 80% dependence on import of domestic agricultural potash fertilizer, agricultural is the important foundation of Chinese national economy and social development, and the potash fertilizer problem has become the bottleneck of China's agricultural sustainable development.
For guaranteeing the particularly security needs of grain of China's agricultural, must implement the development strategy of going global.Therefore, base oneself upon foreign resources, the sylvite Mineral resources of cooperative development surrounding countries are one of main effective ways that fundamentally solve China's potash fertilizer demand, also are the elementary tactics that China must adhere to for a long time.
The technology of utilizing potassium resource to produce Repone K both at home and abroad mainly is divided into four big classes: i.e. flotation technology; Thermosol cold crystallization technology; The dense medium separation technology; The electrostatic separation technology.In the explored sylvite reserves of China, 95% reserves lack large-scale soluble solids sylvite deposit from salt lake brine mineral deposit in the quaternary period, and place's ancient times (tertiary period) solid sylvite deposit is only found in the whole nation.
Laos's sylvite deposit is large-scale soluble solids sylvite deposits in ancient times (tertiary period); extractive technique to its ore-forming element potassium; because special natural environment and environmental protection requirement are arranged, the development and use of Laos's sylvite ore still do not have mature experience to can be used as reference.Therefore, domestic a little less than the technical elements relative thin of utilizing solid Potash Resources production in ancient times Repone K.
Summary of the invention
Technical problem to be solved by this invention provides the method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K of utilizing that a kind of production cost is low, the Repone K yield is high.
For addressing the above problem, a kind of method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K of utilizing of the present invention comprises the steps:
(1) tertiary period solid sylvite raw material ore deposit be crushed to particle diameter less than 1mm after, add mother liquor, obtain slip; The weight ratio of wherein said raw material ore deposit and described mother liquor is 1: 3～4;
(2) in described slip, add flotation reagent, after mixing, by one-level roughly select, one-level is scanned, the one-level cleaning technological flowasheet carries out flotation, obtains flotation concentrate carnallitite, flotation tailings sodium-chlor and decomposition nut liquid after the filtration respectively; Wherein the weight ratio of raw material ore deposit and flotation reagent is 1000: 0.05～0.20;
(3) the flotation concentrate carnallitite of described step (2) gained is carried out decomposition and crystallization by itself and 2.5: 1～3: 1 weight ratio of water after, obtain thick Repone K and decomposition nut liquid;
(4) decomposition nut liquid with described step (3) gained evaporates under 105～110 ℃ of temperature, and after the cooling, solid-liquid separation obtains solid carnallitite and sodium chloride mixture and secondary mother liquid under the room temperature; Described mixture returns in the described step (2) and carries out flotation; Described secondary mother liquid then evaporates under 124～146 ℃ of temperature, all is converted into magnesium chloride product after the cooling under the room temperature;
(5) described thick Repone K is obtained pulp liquor and Repone K through washing and starching after washing, filtering again again, the decomposition process that turns back in the described step (3) of pulp liquor utilizes again again, and with after the Repone K drying, obtains the Repone K product of grade＞97%.
Mother liquor in the described step (1) is meant that adding water by raw material ore deposit and 3: 1～3.3: 1 weight ratio of water in the raw material ore deposit decomposes the mixed solution that obtains.
Flotation reagent in the described step (2) is that carbon chain lengths is that 6～20 fatty amide and carbon chain lengths are one or more in 12～20 the alkyl morpholine.
The weight ratio of washing and starching thick Repone K and water when washing, mother liquor again in the described step (5) is 100: 15～25: 150～200.
The present invention compared with prior art has the following advantages:
1, owing to the present invention is directed to Laos's potassium ore deposit characteristics, raw ore is carried out fragmentation, carnallitite and sodium-chlor are dissociated fully, therefore, saved the investment and the running cost of grinding attachment effectively by the simple crushing mode.
2, sodium chloride content is lower than 2.5% in the resulting carnallitite of reverse floatation process because the present invention adopts,, therefore, compare the decomposition course yield height of low-sodium carnalite with similar technology, the product purity height that obtains simultaneously.
3, owing among the present invention decomposition nut liquid is adopted the twice evaporation removal process, make that potassium and the magnesium in the decomposition nut liquid utilizes fully, therefore, three-waste free discharge, compliance with environmental protection requirements.
Embodiment
The example that the present invention produces Repone K with Laos's solid in tertiary period sylvite ore describes in detail.
The raw material ore deposit is Laos's solid in tertiary period sylvite ore test core, diameter 10cm, wherein potassium content 8.20%, magnesium ion content 4.92%, sodium ions content 16.49% in the raw material.
Embodiment utilizes the method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K for 1 one kinds, comprises the steps:
(1) the raw material ore deposit through the hammer mill that mine locating machine works in Wuhan produces be crushed to particle diameter less than 1mm after, get raw ore 750g, in steel basin, add the 2250g mother liquor and size mixing, obtain the 3000g slip.
Wherein mother liquor is meant that adding water by raw material ore deposit and 3: 1 weight ratio of water in the raw material ore deposit decomposes the mixed solution that obtains.
(2) slip is sent into the flotation operation, by adding flotation reagent, wherein the weight ratio of raw material ore deposit and flotation reagent is 1000: 0.05 in slip; After mixing, by one-level roughly select, one-level is scanned, the one-level cleaning technological flowasheet carries out flotation, flotation 5min obtains 447g flotation concentrate carnallitite (wherein containing carnallitite 90.73%), 324g flotation tailings sodium-chlor and 2210g decomposition nut liquid respectively after the SS-300 link-suspended basket centrifuge filters altogether.
Flotation reagent is that carbon chain lengths is 6～20 fatty amide.
(3) carnallitite with step (2) gained adds entry by itself and 2.5: 1 weight ratio of water, and the stirring velocity with 80rpm is carried out decomposition and crystallization in steel basin, and the decomposition reaction time is 20 minutes, and the potassium total recovery is greater than 82%, obtain the thick Repone K of 101g, wherein KCE content is 87.23%.Obtain decomposition nut liquid 557g simultaneously.
(4) decomposition nut liquid with step (3) gained evaporates under 105 ℃ of temperature, is the evaporation terminal point when boiling point reaches 107～108 ℃; After the cooling, solid-liquid separation obtains 136g solid carnallitite and sodium chloride mixture and 330g secondary mother liquid under the room temperature---the saturated mother liquor of magnesium chloride.This mixture returns in the step (2) and carries out flotation; Secondary mother liquid then evaporates under 124 ℃ of temperature, when the solution boiling point reaches 145～146 ℃, for the evaporation terminal point, after the cooling, obtains solid magnesium chloride product 247g under the room temperature.
(5) thick Repone K is put into steel basin, by the weight ratio of thick Repone K and water, mother liquor is to add entry and mother liquor at 100: 15: 150, wash and starch again with the stirring velocity of 80rpm and to wash, washed 20～30 minutes after whizzer obtains 234g pulp liquor and 87g Repone K again after filtering; Will be again the decomposition process that turns back in the step (3) of pulp liquor utilize again, and with Repone K with baking oven behind dry 1～2h under 100～110 ℃ of temperature, obtain the Repone K product of 82.5g, grade＞97%.
Embodiment utilizes the method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K for 2 one kinds, comprises the steps:
(1) the raw material ore deposit through crusher in crushing to particle diameter less than 1mm after, get raw ore 750g, in steel basin, add the 3000g mother liquor and size mixing, obtain the 3750g slip.
Wherein mother liquor is meant that adding water by raw material ore deposit and 3.3: 1 weight ratio of water in the raw material ore deposit decomposes the mixed solution that obtains.
(2) slip is sent into the flotation operation, by adding flotation reagent, wherein the weight ratio of raw material ore deposit and flotation reagent is 1000: 0.20 in slip; After mixing, by one-level roughly select, one-level is scanned, the one-level cleaning technological flowasheet carries out flotation, flotation 5min obtains 443g flotation concentrate carnallitite (wherein containing carnallitite 90.50%), 331g flotation tailings sodium-chlor and 3030g decomposition nut liquid respectively after whizzer filters altogether.
Flotation reagent is that carbon chain lengths is 12～20 alkyl morpholine.
(3) carnallitite with step (2) gained adds entry by itself and 3: 1 weight ratio of water, and the stirring velocity with 80rpm is carried out decomposition and crystallization in steel basin, and the decomposition reaction time is 20 minutes, and the potassium total recovery is greater than 83%, obtain the thick Repone K of 105g, wherein KCE content is 83.32%.Obtain decomposition nut liquid 542g simultaneously.
(4) decomposition nut liquid with step (3) gained evaporates under 110 ℃ of temperature, is the evaporation terminal point when boiling point reaches 107～108 ℃; After the cooling, solid-liquid separation obtains 130g solid carnallitite and sodium chloride mixture and 321g secondary mother liquid under the room temperature---the saturated mother liquor of magnesium chloride.This mixture returns in the step (2) and carries out flotation; Secondary mother liquid then evaporates under 146 ℃ of temperature, when the solution boiling point reaches 145～146 ℃, for the evaporation terminal point, after the cooling, obtains solid magnesium chloride product 232g under the room temperature.
(5) thick Repone K is put into steel basin, by the weight ratio of thick Repone K and water, mother liquor is to add entry and mother liquor at 100: 25: 200, wash and starch again with the stirring velocity of 80rpm and to wash, washed 20～30 minutes after whizzer obtains 243g pulp liquor and 85g Repone K again after filtering; Will be again the decomposition process that turns back in the step (3) of pulp liquor utilize again, and with Repone K with baking oven behind dry 1～2h under 100～110 ℃ of temperature, obtain the Repone K product of 79.1g, grade＞97%.
Embodiment utilizes the method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K for 3 one kinds, comprises the steps:
(1) the raw material ore deposit through crusher in crushing to particle diameter less than 1mm after, get raw ore 750g, in steel basin, add the 2625g mother liquor and size mixing, obtain the 3375g slip.
Wherein mother liquor is meant that adding water by raw material ore deposit and 3.2: 1 weight ratio of water in the raw material ore deposit decomposes the mixed solution that obtains.
(2) slip is sent into the flotation operation, by adding flotation reagent, wherein the weight ratio of raw material ore deposit and flotation reagent is 1000: 0.13 in slip; After mixing, by one-level roughly select, one-level is scanned, the one-level cleaning technological flowasheet carries out flotation, flotation 5min obtains 456g flotation concentrate carnallitite (wherein containing carnallitite 91.01%), 340g flotation tailings sodium-chlor and 2220g decomposition nut liquid respectively after whizzer filters altogether.
Flotation reagent is that carbon chain lengths is that 6～20 fatty amide and carbon chain lengths are 12～20 alkyl morpholine mixture, and wherein the volume ratio of fatty amide and alkyl morpholine is 1～2: 0.5.
(3) carnallitite with step (2) gained adds entry by itself and 2.8: 1 weight ratio of water, and the stirring velocity with 80rpm is carried out decomposition and crystallization in steel basin, and the decomposition reaction time is 20 minutes, and the potassium total recovery is greater than 82%, obtain the thick Repone K of 104g, wherein KCE content is 87.13%.Obtain decomposition nut liquid 556g simultaneously.
(4) decomposition nut liquid with step (3) gained evaporates under 107 ℃ of temperature, is the evaporation terminal point when boiling point reaches 107～108 ℃; After the cooling, solid-liquid separation obtains 133g solid carnallitite and sodium chloride mixture and 322g secondary mother liquid under the room temperature---the saturated mother liquor of magnesium chloride.This mixture returns in the step (2) and carries out flotation; Secondary mother liquid then evaporates under 135 ℃ of temperature, when the solution boiling point reaches 145～146 ℃, for the evaporation terminal point, after the cooling, obtains solid magnesium chloride product 239g under the room temperature.
(5) thick Repone K is put into steel basin, by the weight ratio of thick Repone K and water, mother liquor is to add entry and mother liquor at 100: 20: 175, wash and starch again with the stirring velocity of 80rpm and to wash, washed 20～30 minutes after whizzer obtains 239g pulp liquor and 89g Repone K again after filtering; Will be again the decomposition process that turns back in the step (3) of pulp liquor utilize again, and with the Repone K baking oven behind dry 1～2h under 100～110 ℃ of temperature, obtain the Repone K product of 84g, grade＞97%.
Claims (4)
1. one kind is utilized the method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K, comprises the steps:
(1) tertiary period solid sylvite raw material ore deposit be crushed to particle diameter less than 1mm after, add mother liquor, obtain slip; The weight ratio of wherein said raw material ore deposit and described mother liquor is 1: 3～4;
(2) in described slip, add flotation reagent, after mixing, by one-level roughly select, one-level is scanned, the one-level cleaning technological flowasheet carries out flotation, obtains flotation concentrate carnallitite, flotation tailings sodium-chlor and decomposition nut liquid after the filtration respectively; Wherein the weight ratio of raw material ore deposit and flotation reagent is 1000: 0.05～0.20;
(3) the flotation concentrate carnallitite of described step (2) gained is carried out decomposition and crystallization by itself and 2.5: 1～3: 1 weight ratio of water after, obtain thick Repone K and decomposition nut liquid;
(4) decomposition nut liquid with described step (3) gained evaporates under 105～110 ℃ of temperature, and after the cooling, solid-liquid separation obtains solid carnallitite and sodium chloride mixture and secondary mother liquid under the room temperature; Described mixture returns in the described step (2) and carries out flotation; Described secondary mother liquid then evaporates under 124～146 ℃ of temperature, all is converted into magnesium chloride product after the cooling under the room temperature;
(5) described thick Repone K is obtained pulp liquor and Repone K through washing and starching after washing, filtering again again, the decomposition process that turns back in the described step (3) of pulp liquor utilizes again again, and with after the Repone K drying, obtains the Repone K product of grade＞97%.
2. a kind of method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K of utilizing as claimed in claim 1, it is characterized in that: the mother liquor in the described step (1) is meant that adding water by raw material ore deposit and 3: 1～3.3: 1 weight ratio of water in the raw material ore deposit decomposes the mixed solution that obtains.
3. a kind of method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K of utilizing as claimed in claim 1 is characterized in that: the flotation reagent in the described step (2) is that carbon chain lengths is that 6～20 fatty amide and carbon chain lengths are one or more in 12～20 the alkyl morpholine.
4. a kind of method that the tertiary period, solid sylvite ore inverse flotation method was produced Repone K of utilizing as claimed in claim 1 is characterized in that: the weight ratio of washing and starching thick Repone K and water when washing, mother liquor again in the described step (5) is 100: 15～25: 150～200.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167362A (en) * | 2011-03-22 | 2011-08-31 | 天津长芦汉沽盐场有限责任公司 | Potassium chloride production process for decomposing carnallite with cleaning solution |
| CN112007751A (en) * | 2019-12-16 | 2020-12-01 | 中蓝连海设计研究院有限公司 | Method for treating potassium mixed salt type ore by adopting dense medium and cold crystallization direct flotation |
| CN115215355A (en) * | 2022-08-19 | 2022-10-21 | 中国科学院青海盐湖研究所 | Method for reducing fine sodium chloride in potassium chloride product and application thereof |
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2009
- 2009-12-24 CN CN2009101177629A patent/CN101723408B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167362A (en) * | 2011-03-22 | 2011-08-31 | 天津长芦汉沽盐场有限责任公司 | Potassium chloride production process for decomposing carnallite with cleaning solution |
| CN112007751A (en) * | 2019-12-16 | 2020-12-01 | 中蓝连海设计研究院有限公司 | Method for treating potassium mixed salt type ore by adopting dense medium and cold crystallization direct flotation |
| CN115215355A (en) * | 2022-08-19 | 2022-10-21 | 中国科学院青海盐湖研究所 | Method for reducing fine sodium chloride in potassium chloride product and application thereof |
| CN115215355B (en) * | 2022-08-19 | 2024-02-23 | 中国科学院青海盐湖研究所 | Method for reducing fine sodium chloride in potassium chloride product and application thereof |
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