CN1314308A - Method for preparing potassium sulfate by one section conversion flotation process - Google Patents
Method for preparing potassium sulfate by one section conversion flotation process Download PDFInfo
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- CN1314308A CN1314308A CN 01118069 CN01118069A CN1314308A CN 1314308 A CN1314308 A CN 1314308A CN 01118069 CN01118069 CN 01118069 CN 01118069 A CN01118069 A CN 01118069A CN 1314308 A CN1314308 A CN 1314308A
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- tartar
- agent
- vitriolate
- flotation
- mixture
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Abstract
The converting floatation process includes mixing salina carnallite and/or potassium mineral with natural mirabilite in the stoichiometric ratio of 1.0-1.2 to 1.0, adding sufficient circular mother liquod for conversion at 5-90 deg.c, adding floating agent into the ore pulp material for floatation, centrifugally separating floated ore pulp to obtain potassium sulfate and returning centrifugal mother liquor into the technological process. The process of the present invention can utilize mother liquor circularly and may use potassium mineral with low potassium content, such as crude potassium obtained by decomposing salina cernalite, and low content mirabilite.
Description
The invention belongs to the inorganic salt field, particularly a kind of method of preparing potassium sulfate by one section conversion flotation process.
At present, the method for producing vitriolate of tartar generally all adopts with vitriol (Na
2SO
4MgSO
4H
2SO
4) and Repone K (KCl) be raw material, the Technology of carrying out two sections conversion reactions.This method is to the purity requirement height of use raw material, and the technology mother liquor can not recycle, and needs evaporation to reclaim useful salt, and the course of processing is longer, and energy consumption is more, and manufacturing cost is also high.For example, disclose a kind of manufacture method of vitriolate of tartar among the CN1086017, this method adopts the technology of twice transformation, single vaporization, makes sodium sulfate and Repone K change into vitriolate of tartar.
It is the Technology of utilizing collecting agent to carry out flotation that the preparation vitriolate of tartar also has a kind of method, is two sections conversion methods of raw material but also be detected in high purity saltcake and Repone K, promptly to glaserite (3K
2SO
4Na
2SO
4) carry out flotation.The Technology that another kind utilizes collecting agent to carry out flotation is to be two sections conversion methods of raw material with sal epsom and Repone K, promptly to schoenite (K
2SO
4MgSO
4) carry out flotation.CN1089575 discloses a kind of method that adopts extraction process to produce vitriolate of tartar, this method is to put into extraction tank with the sal enixum that wet processing makes, sal enixum is dissolved in extraction and returns in feed liquid and the water, add the Repone K that purifies, and adding fat tertiary amine kind of extractants, material layering, lower floor is a vitriolate of tartar.Adopt this method to need the Repone K purity height that is adopted, and productive rate is not high.
The object of the present invention is to provide a kind of method of preparing potassium sulfate by one section conversion flotation process, in order to overcome the above-mentioned defective that ordinary method is produced when preparing vitriolate of tartar.This method can make the technology Recycling Mother Solution use, and can use to contain thick potassium (low-grade potash fertilizer) and the natural saltcake of low levels that the low potassium mineral of potassium, salt pan photolysis obtain and be raw material.
The method of preparing potassium sulfate by one section conversion flotation process of the present invention comprises: with salt pan carnallitite or potassium mineral or the mixture of the two and natural saltcake by 1.0～1.2 of stoichiometric quantity: 1.0 mix, the circulating mother liquor that adds q.s, under 5～90 ℃ temperature, transform, in this ore pulp material, add flotation agent again, the ore pulp material that has added flotation agent is carried out flotation, the ore pulp that floatingly selects just obtains vitriolate of tartar through centrifugation, and centrifuge mother liquor returns the technological process circulation.
Specifically describe the procedure that the present invention prepares vitriolate of tartar below.
Step 1: transform, when being raw material, at first in the light stone of salt pan, adding water and carry out cold decomposition, obtain thick potassium (low-grade potash fertilizer) with the salt pan carnallitite.And when being raw material with the potassium mineral, can directly use.With thick potassium and natural saltcake according to 1.0～1.2 of stoichiometric quantity: 1.0 mix, mixture is put in the conversion vessel that has agitator, the circulating mother liquor that adds q.s, making pulp density is 30～50% (weight), under 5～90 ℃ temperature, stir with 60 rev/mins～120 rev/mins rotating speeds, carry out conversion reaction, transform and generate the vitriolate of tartar precipitation, conversion reaction was carried out 0.7～2.0 hour;
Step 2: flotation, in the ore pulp material that step 1 obtains, add flotation agent, flotation agent is collecting agent and the mixture of adjusting agent.Collecting agent is C6～C14 alkylsulfonate, C6～C18 alkyl trimethyl Sodium Bromide or the mixture of the two, and the add-on of collecting agent is 150～450g/T
K2SO4Adjusting agent is the mixture of inclined to one side sodium polyphosphate, yellow soda ash and water glass, and add-on is 250～500g/T
K2SO4
Collecting agent that this step adopts is preferably C6～C14 alkyl sodium sulfonate, further preferred C8～C10 alkyl sodium sulfonate.C6 in the collecting agent～C14 alkylsulfonate and C6～C18 alkyl trimethyl Sodium Bromide can be with any mixed, preferred C6～C14 alkylsulfonate: C6～C18 alkyl trimethyl Sodium Bromide=3～10: 1 (weight ratio), further preferred 4～6: 1.Inclined to one side sodium polyphosphate, yellow soda ash and the water glass adjusted in the agent can be with any mixed, preferred sodium polyphosphate partially: yellow soda ash: water glass=2: 1: 1 (weight ratio).
Step 3: with the adding of step 2 the ore pulp material of flotation agent carry out flotation, can send in the bubble cell and roughly select, scan with selected;
Step 4: the selected foam ore pulp that obtains is through the whizzer solid-liquid separation, and the wet basis vitriolate of tartar after the drying dehydration, obtains the finished product vitriolate of tartar with the water washing of 0.5～2.0 times of amount then; Centrifuge mother liquor and washing water return technological process and recycle, and flotation tailings is the sodium chloride as impurity that contains sludge.
The advantage of the inventive method is that existing two sections conversions are become one section conversion, and the technology Recycling Mother Solution is used, and having shortened flow process greatly, can use to contain the low potassium mineral of potassium, decompose the thick potassium (low-grade potash fertilizer) that obtains as the salt pan carnallitite, also can use the natural saltcake of low levels to be raw material.
Further describe technical scheme of the present invention below in conjunction with embodiment and accompanying drawing.
Fig. 1. the present invention transforms the process flow diagram that flotation process prepares vitriolate of tartar for one section.
Embodiment 1
Take by weighing salt pan carnallitite (containing KCl18.14%) 10.0Kg, add water 4.5Kg, at room temperature stir and decomposed 15 minutes, obtain thick potassium 3.9Kg after the solid-liquid separation, take by weighing thick potassium 370g, natural saltcake (contains Na
2SO
476.20%) 185g contains in the 2000ml beaker, adds the 840g mother liquor, at 17.5 ℃, and under 80 rev/mins of the mixing speed, conversion reaction 1.5 hours; Add collecting agent and adjust agent to slip, 28 milligrams of 58 milligrams of collecting agent employing C10 alkyl sodium sulfonates and C1O alkyl trimethyl Sodium Bromides, adjust agent and adopt 18 milligrams of 35 milligrams of inclined to one side sodium polyphosphates, 18 milligrams in yellow soda ash and water glass, put into then during flotation meets with, behind the air flotation 7 minutes, the froth concentrate centrifugation, the wet basis product gets wet basis K with 500g water washing 3 times
2SO
4Product 183.0g carries out drying under 108 ℃, obtain vitriolate of tartar, and its chemical composition is as follows:
K
+?40.85％,SO
4 2-?50.15％,Cl
-?2.36％.
K in the sample
2O=49.21%, the potassium rate of recovery is 64.24%, the rate of recovery of sulfate radical is 85.24%.
Embodiment 2:
Take by weighing natural potassium mineral (containing KCl19.20%) 1000g and natural saltcake (Na
2SO
493.0%) 195g, contain in the 5000ml beaker, add mother liquor 1900g, under 31 ℃, under 90 rev/mins of conditions of mixing speed, conversion reaction 1.0 hours, add collecting agent in the slip and adjust agent, 22 milligrams of 48 milligrams of collecting agent employing C8 alkyl sodium sulfonates and C8 alkyl trimethyl Sodium Bromides, adjust agent and adopt 14 milligrams of 27 milligrams of inclined to one side sodium polyphosphates, 14 milligrams in yellow soda ash and water glass, put into then in three liters of flotation cells, through air flotation after 7 minutes, the froth concentrate centrifugation is also used the 700g water washing, gets the wet basis product K
2SO
4235.0g through 102 ℃ of dryings, butt product chemical composition is as follows:
K
+?40.34％,SO
4 2-?49.52％,Cl
-?2.44％
K in the sample
2O=4g.59%, the potassium rate of recovery is 83.38%, the sulfate radical rate of recovery is 84.01%.
Embodiment 3:
Take by weighing thick potassium (KCl40.83%) 268g and natural saltcake (Na
2SO
474.80%) 162g, contain in beaker, add mother liquor 1000g, under 13 ℃, conversion reaction is 2.0 hours under 100 rev/mins of conditions of mixing speed, slip adds collecting agent and adjusts agent, 23 milligrams of 48 milligrams of collecting agent employing C12 alkyl sodium sulfonates and C12 alkyl trimethyl Sodium Bromides are adjusted agent and are adopted 29 milligrams of inclined to one side sodium polyphosphates, 15 milligrams of 15 milligrams in yellow soda ash and water glass are put in the flotation cell then, through abundant flotation after 6.5 minutes, the froth concentrate centrifugation, and, get wet basis product 156g with 300g water washing three times, dry under 102 ℃ temperature, the chemical composition of butt product is as follows:
K
+?41.85％,SO
4 2-?51.38％,Cl
-?1.91％
K in the sample
2O=50.41%, the potassium rate of recovery is 84.1%, the sulfate radical rate of recovery is 85.37%.
Claims (7)
1. one kind one section transforms the method that flotation process is produced vitriolate of tartar, it is characterized in that: this method be with salt pan carnallitite or potassium mineral or the mixture of the two and natural saltcake by 1.0～1.2 of stoichiometric quantity: 1.0 mix, the circulating mother liquor that in mixture, adds q.s, under 5～90 ℃ temperature, transform, in this ore pulp material, add flotation agent again, the ore pulp material that has added flotation agent is carried out flotation, the ore pulp that floatingly selects just obtains the product vitriolate of tartar through centrifugation, and centrifuge mother liquor returns the technological process circulation.
2. the method for the production vitriolate of tartar of claim 1 record, it is characterized in that: described flotation agent is collecting agent and the mixture of adjusting agent, and collecting agent is C6～C14 alkyl sodium sulfonate, C6～C18 alkyl trimethyl Sodium Bromide or the mixture of the two; Adjusting agent is the mixture of inclined to one side sodium polyphosphate, yellow soda ash and water glass.
3. the method for production vitriolate of tartar of claim 1 or 2 records, it is characterized in that: described collecting agent is C8～C10 alkyl sodium sulfonate and C10～14 alkyl trimethyl Sodium Bromides.
4. the method for the production vitriolate of tartar of claim 1 record, it is characterized in that: the weight ratio of alkyl sodium sulfonate and alkyl trimethyl Sodium Bromide is 4～6: 1 in the described collecting agent.
5. the method for the production vitriolate of tartar of claim 1 record, it is characterized in that: the add-on of described collecting agent is 150～450g/T
K2SO4, the add-on of adjusting agent is 250～500g/T
K2SO4
6. the method for the production vitriolate of tartar of claim 1 record, it is characterized in that: described conversion is to carry out under 5～90 ℃ temperature.
7. the method for the production vitriolate of tartar of claim 1 record, it is characterized in that: it is 30～50% (weight) that the mother liquor amount that adds in the mixture should make pulp density.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011180692A CN1156396C (en) | 2001-05-18 | 2001-05-18 | Method for preparing potassium sulfate by one section conversion flotation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011180692A CN1156396C (en) | 2001-05-18 | 2001-05-18 | Method for preparing potassium sulfate by one section conversion flotation process |
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| Publication Number | Publication Date |
|---|---|
| CN1314308A true CN1314308A (en) | 2001-09-26 |
| CN1156396C CN1156396C (en) | 2004-07-07 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102476076A (en) * | 2010-11-25 | 2012-05-30 | 何建庭 | New purpose of primary and secondary alkyl sodium sulfonate |
| CN102626674A (en) * | 2012-04-12 | 2012-08-08 | 中国科学院青海盐湖研究所 | Method for extracting vesuvius salt from carbonate saline lake |
| CN101474598B (en) * | 2009-01-23 | 2012-10-24 | 云南省化工研究院 | Method for flotation of potassium chloride from potassium salt mine |
| CN110198921A (en) * | 2016-12-17 | 2019-09-03 | 死海工程有限公司 | By the method for carnallite and sodium sulphate production sulphate of potash and magesium |
-
2001
- 2001-05-18 CN CNB011180692A patent/CN1156396C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101474598B (en) * | 2009-01-23 | 2012-10-24 | 云南省化工研究院 | Method for flotation of potassium chloride from potassium salt mine |
| CN102476076A (en) * | 2010-11-25 | 2012-05-30 | 何建庭 | New purpose of primary and secondary alkyl sodium sulfonate |
| CN102626674A (en) * | 2012-04-12 | 2012-08-08 | 中国科学院青海盐湖研究所 | Method for extracting vesuvius salt from carbonate saline lake |
| CN110198921A (en) * | 2016-12-17 | 2019-09-03 | 死海工程有限公司 | By the method for carnallite and sodium sulphate production sulphate of potash and magesium |
| US11306033B2 (en) | 2016-12-17 | 2022-04-19 | Dead Sea Works Ltd. | Process for the production of potassium sulphate and magnesium sulphate from carnallite and sodium sulphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1156396C (en) | 2004-07-07 |
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