CN104998748A - Technology for extracting potassium and removing sodium from high-sodium polyhalite ore - Google Patents

Technology for extracting potassium and removing sodium from high-sodium polyhalite ore Download PDF

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Publication number
CN104998748A
CN104998748A CN201510342985.0A CN201510342985A CN104998748A CN 104998748 A CN104998748 A CN 104998748A CN 201510342985 A CN201510342985 A CN 201510342985A CN 104998748 A CN104998748 A CN 104998748A
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CN
China
Prior art keywords
sodium
flotation
polyhalite
mother liquor
potassium
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CN201510342985.0A
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Chinese (zh)
Inventor
季荣
甘顺鹏
胡勇
冯文平
谭之海
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China Bluestar Chonfar Engineering and Technology Co Ltd
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China Bluestar Changsha Design and Research Institute
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Priority to CN201510342985.0A priority Critical patent/CN104998748A/en
Publication of CN104998748A publication Critical patent/CN104998748A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated

Abstract

A technology for extracting potassium and removing sodium from high-sodium polyhalite ore includes the following steps that firstly, the high-sodium polyhalite ore is ground; secondly, flotation mother liquor returns to a closed technological process in the sequence of one-time roughing, two-time concentration, one-time scavenging, returning of middlings in concentration I and scavenged concentrate to roughing, and returning of middlings in the concentration II to concentration I, wherein 100-200 g/ton anionic collectors are added in the roughing process, flotation time ranges from 3 minutes to 5 minutes, 50-100 g/ton anionic collectors are added in the scavenging process, flotation time ranges from 2 minutes to 3 minutes, no collectors are added in the process of the two-time concentration, flotation time ranges from 3 minutes to 5 minutes, and flotation concentrate can be obtained; and thirdly, the flotation concentrate is washed and filtered, and low-sodium polyhalite is obtained. The technology is reasonable in process; the flotation technology is mature and reliable; the process and the reagent rule are simple; the technology is low in investment, easy to operate, low in energy and water consumption and low in comprehensive production cost; and large-scale industrial production can be achieved easily.

Description

A kind of potassium of carrying from high sodium polyhalite is except the technique of sodium
Technical field
The present invention relates to a kind of potassium of carrying from high sodium polyhalite except the technique of sodium, be specifically related to a kind of mode by direct flotation-washing from high sodium polyhalite, extract the technique obtaining low sodium polyhalite.
Background technology
Polyhalite (K 2sO 4mgSO 42CaSO 42H 2o) be a kind of containing potassium magnesiumsulphate double salt mineral, the solubility in water is very little.This ore deposit is composed and is stored in steam curing rock, and being a kind of paragenous mineral, is the refractory potassic mine stone be extensively distributed in sulfate type sylvite deposit, its K 2o theoretical content reaches 15.64%.But because its poorly water-soluble and ore body bury comparatively dark, production technique difficulty is comparatively large, so be regarded as slow-witted ore deposit for a long time and be not utilized.Therefore, research and development polyhalite, to the Chinese potassium deficiency present situation of change, development potash fertilizer industry important in inhibiting.
Polyhalite resource is very abundant, can be divided into high sodium polyhalite and low sodium polyhalite by gangue mineral (sodium chloride) content height.At present, developmental research for low sodium polyhalite is more, reported process route has calcining molten leaching, acidolysis, molten leaching etc., and wherein the U.S.'s intercontinental potash fertilizer company utilizes calcining leaching technology process low sodium polyhalite preparing potassium sulfate exactly, obtains good effect.
At present, domestic and international polyhalite treatment process can be divided into following a few class:
The first kind: sylvite is produced in acidolysis, namely utilizes the highly acid material acidolysis polyhalites such as nitric acid, makes it decompose, then reclaim sylvite from decomposed solution.CN102869609A discloses and uses HNO 3react with polyhalite and generate containing potassium solution, then add Ca (OH) 2, then prepare KNO through links such as fractional crystallizations 3method; US1946068 and US4246019 also discloses and utilizes HNO 3the method of sylvite prepared by process polyhalite; RU2276123 discloses a kind of HNO 3react with polyhalite, then contain K with in ammonia with preparation 2sO 4, MgSO 4and NH 4nO 3the method of mixture solution.
Equations of The Second Kind: calcining Hydrolyze method, polyhalite is crushed to certain particle size, and high-temperature calcination destroys its mineral structure, changes its dissolution properties, then the useful element be dissolved in water wherein is recycled.CN102596856A adds water after disclosing and being calcined by polyhalite, forms syngenite, then reacts with alkaline Ca compound, preparation KNO 3method; US2138827 calcines with sodium nitrate molten after disclosing and polyhalite being crushed to 10-20 order, then the water-soluble method preparing sulfur acid potassium solution; Intercontinental potash fertilizer company of the U.S. has applied for the Patents of polyhalite, and such as it just describes the method utilizing calcining Hydrolyze method processing polyhalite to prepare potassium sulfate at the patent CN103930371A of China's application.
3rd class: molten leaching method, the method removes molten leaching polyhalite with certain special solution as leachant, and useful element in polyhalite is entered in solution.US1981125 discloses polyhalite and reacts with the limewash of heat the method preparing potassium sulfate; US1956930 discloses and polyhalite and lime stone is reacted the method preparing potassium sulfate in airtight container; CN1045755A disclose utilize common-ion effect with 3.5% potassium sulfate solution from gypsum, polyhalite mixed ore, extract the method for potassium sulfate, magnesium sulfate, calcium sulfate; Also have some bibliographical informations about the exploitation of deep polyhalite, principle is also molten leaching method, as CN1766138A discloses a kind of production by dissolving and leaching process method to potassium in polyhalite, proposes and adopts CaCl 2deng the aqueous solution as leaching solution, production by dissolving and leaching process is carried out to the potassium in polyhalite, and point out that the polyhalite that namely the method can be used for descending the degree of depth to bury over the ground carries out Situ Leaching exploitation, be also applicable to carry out dump leaching process to earth's surface or shallow polyhalite potash ore deposit.
The process route that above-mentioned patent and document adopt is all for low sodium polyhalite or pure polyhalite, and has no relevant report to the exploitation of high sodium polyhalite (NaCl mass percentage >=10%).
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of from high sodium polyhalite, puies forward the technique of potassium except sodium.
The technical solution adopted for the present invention to solve the technical problems is: a kind of potassium of carrying from high sodium polyhalite, except the technique of sodium, comprises the following steps:
(1) the high sodium polyhalite ore grinding of mass percent >=10% of NaCl in raw ore to-150 orders (-0.106mm) are accounted for 75wt%-85wt%;
(2) in flotation mother liquor, one roughing is adopted, twice selected, once purging selection, selected I chats, scavenger concentrate returns to be roughly selected, the order of selected II middling recurrence selected I returns closed circuit technological process, roughly selecting concentration is the preferred 30wt% of 25wt%-35wt%(), scanning concentration is the preferred 20wt% of 15wt%-25wt%(), roughly select and add anionic collector 100-200 gram/ton, flotation time is 3-5 minute, scan and add anionic collector 50-100 gram/ton, flotation time is 2-3 minute, selected selected for not adding collecting agent twice, flotation time is all 3-4 minute, obtain flotation concentrate,
(3) flotation concentrate washing, filters, obtains low sodium polyhalite.
Further, in step (1), grinding mode is ball milling, and ore grinding mass concentration is 50%-65%, and milling medium is the saturated mother liquor of NaCl.
Further, in step (2), described flotation mother liquor is the saturated mother liquor of NaCl, and Recycling Mother Solution uses.
Further, in step (2), described anionic collector is alkylsulfonate or alkyl sulfate, and its alkyl carbon chain lengths is 10-16.
Further, in step (3), washing used medium is the mixed liquor of flotation mother liquor and water.Wherein, flotation mother liquor is sized mixing use.
Further, in step (3), the mass ratio of flotation concentrate, flotation mother liquor and water is 10:8-10:1.5-2.0.
The present invention with high sodium polyhalite for raw material, extract polyhalite by direct flotation-washing process and remove sodium chloride, produce potash fertilizer technique for subsequent treatment polyhalite and qualified low sodium polyhalite is provided, whole technological process is simple, have investment little, easy and simple to handle, energy, water consumption is low, comprehensive production cost is low, is easy to realize the advantages such as large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the process chart of the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
embodiment 1
The present embodiment comprises the following steps:
(1) by high sodium polyhalite (K 2sO 4mgSO 42CaSO 42H 2o content 60.12wt%, NaCl content 34.22wt%) ore grinding accounts for 81.21wt% to-150 orders (-0.106mm), and grinding mode is ball milling, and ore grinding mass concentration is 50%, and milling medium is the saturated mother liquor of NaCl;
(2) in the saturated mother liquor of NaCl, adopt one roughing, twice selected, once purging selection, and selected I chats, scavenger concentrate return and roughly select, and the order of selected II middling recurrence selected I returns closed circuit technological process, and roughly selecting concentration is 29wt%, scans concentration 21wt%; Roughly select and add anionic collector dodecyl sodium sulfate 150 grams/ton, flotation time is 4 minutes, scans and adds anionic collector dodecyl sodium sulfate 75 grams/ton, and flotation time is 3 minutes, selected selected for not adding collecting agent twice, flotation time is all 4 minutes; Obtain flotation concentrate, K in flotation concentrate 2sO 4mgSO 42CaSO 42H 2o content 83.25wt%, NaCl content 4.41wt%, K +the rate of recovery 92.62%;
(3) flotation concentrate washing, using the mixed liquor of flotation mother liquor and water as washing medium, wherein, the mass ratio of flotation concentrate, flotation mother liquor and water is 10:8:2, then filters, result of the test: can obtain K 2sO 4mgSO 42CaSO 42H 2the low sodium polyhalite concentrate of O content 92.13wt%, NaCl content 0.398wt%, K +the rate of recovery 97.72%.
embodiment 2
The present embodiment comprises the following steps:
(1) by high sodium polyhalite (K 2sO 4mgSO 42CaSO 42H 2o content 76.72wt%, NaCl content 16.32wt%) ore grinding accounts for 83.20wt% to-150 orders (-0.106mm), and grinding mode is ball milling, and ore grinding mass concentration is 60%, and milling medium is the saturated mother liquor of NaCl;
(2) in the saturated mother liquor of NaCl, adopt one roughing, twice selected, once purging selection, selected I chats, scavenger concentrate return and roughly select, and the order of selected II middling recurrence selected I returns closed circuit technological process, roughly selecting concentration is 30.02wt%, scans concentration 21.23wt%; Roughly select and add anionic collector sodium cetanesulfonate 180 grams/ton, flotation time is 4 minutes, scans and adds anionic collector sodium cetanesulfonate 75 grams/ton, and flotation time is 3 minutes, selected selected for not adding collecting agent twice, flotation time is all 4 minutes; Obtain flotation concentrate, K in flotation concentrate 2sO 4mgSO 42CaSO 42H 2o content 88.18wt%, NaCl content 3.87wt%, K +the rate of recovery 92.14%;
(3) flotation concentrate washing, using the mixed liquor of flotation mother liquor and water as washing medium, wherein, the mass ratio of flotation concentrate, flotation mother liquor and water is 10:8:2, then filters, result of the test: can obtain K 2sO 4mgSO 42CaSO 42H 2the low sodium polyhalite concentrate of O content 94.21wt%, NaCl content 0.346wt%, K +the rate of recovery 98.01%.
embodiment 3
The present embodiment comprises the following steps:
(1) by high sodium polyhalite (K 2sO 4mgSO 42CaSO 42H 2o content 52.99wt%, NaCl content 41.23wt%) ore grinding accounts for 78.83wt% to-150 orders (-0.106mm), and grinding mode is ball milling, and ore grinding mass concentration is 65%, and milling medium is the saturated mother liquor of NaCl;
(2) in the saturated mother liquor of NaCl, adopt one roughing, twice selected, once purging selection, selected I chats, scavenger concentrate return and roughly select, and the order of selected II middling recurrence selected I returns closed circuit technological process, roughly selecting concentration is 30.01wt%, scans concentration 21.42wt%; Roughly select and add anionic collector lauryl sodium sulfate 125 grams/ton, flotation time is 3 minutes, scans and adds anionic collector lauryl sodium sulfate 50 grams/ton, and flotation time is 3 minutes, selected selected for not adding collecting agent twice, flotation time is all 4 minutes; Obtain flotation concentrate, K in flotation concentrate 2sO 4mgSO 42CaSO 42H 2o content 82.08wt%, NaCl content 4.87wt%, K +the rate of recovery 90.67%;
(3) flotation concentrate washing, using the mixed liquor of flotation mother liquor and water as washing medium, wherein, the mass ratio of flotation concentrate, flotation mother liquor and water is 10:8:2, then filters, result of the test: can obtain K 2sO 4mgSO 42CaSO 42H 2the low sodium polyhalite concentrate of O content 93.12wt%, NaCl content 0.245wt%, K +the rate of recovery 96.99%.
embodiment 4
The present embodiment comprises the following steps:
(1) by high sodium polyhalite (K 2sO 4mgSO 42CaSO 42H 2o content 52.99wt%, NaCl content 41.23wt% ore grinding to-150 orders (-0.106mm) account for 79.34wt%, and grinding mode is ball milling, and ore grinding mass concentration is 50%, and milling medium is the saturated mother liquor of NaCl;
(2) in the saturated mother liquor of NaCl, adopt one roughing, twice selected, once purging selection, selected I chats, scavenger concentrate return and roughly select, and the order of selected II middling recurrence selected I returns closed circuit technological process, roughly selecting concentration is 30.01wt%, scans concentration 21.42wt%; Roughly select and add anionic collector sodium hexadecyl sulfate 150 grams/ton, flotation time is 3 minutes, scans and adds anionic collector sodium hexadecyl sulfate 75 grams/ton, and flotation time is 3 minutes, selected selected for not adding collecting agent twice, flotation time is all 4 minutes; Obtain flotation concentrate, K in flotation concentrate 2sO 4mgSO 42CaSO 42H 2o content 79.87wt%, NaCl content 6.12wt%, K +the rate of recovery 92.67%;
(3) flotation concentrate washing, using the mixed liquor of flotation mother liquor and water as washing medium, wherein, the mass ratio of flotation concentrate, flotation mother liquor and water is 10:8:2, then filters, result of the test: can obtain K 2sO 4mgSO 42CaSO 42H 2the low sodium polyhalite concentrate of O content 93.21wt%, NaCl content 0.213wt%, K +the rate of recovery 96.46%.

Claims (6)

1. from high sodium polyhalite, put forward the technique of potassium except sodium, it is characterized in that, comprise the following steps:
(1) the high sodium polyhalite ore grinding of mass percent >=10% of NaCl in raw ore to-150 orders are accounted for 75wt%-85wt%;
(2) in flotation mother liquor, one roughing is adopted, twice selected, once purging selection, selected I chats, scavenger concentrate return and roughly select, the order of selected II middling recurrence selected I returns closed circuit technological process, roughly selecting concentration is 25wt%-35wt%, scanning concentration is 15wt%-25wt%, roughly select and add anionic collector 100-200 gram/ton, flotation time is 3-5 minute, scans and adds anionic collector 50-100 gram/ton, flotation time is 2-3 minute, selected selected for not adding collecting agent twice, flotation time is all 3-4 minute, obtains flotation concentrate;
(3) flotation concentrate washing, filters, obtains low sodium polyhalite.
2. potassium of carrying from high sodium polyhalite according to claim 1 is except the technique of sodium, and it is characterized in that: in step (1), grinding mode is ball milling, and ore grinding mass concentration is 50%-65%, and milling medium is the saturated mother liquor of NaCl.
3. potassium of carrying from high sodium polyhalite according to claim 1 and 2 is except the technique of sodium, and it is characterized in that: in step (2), described flotation mother liquor is the saturated mother liquor of NaCl, and Recycling Mother Solution uses.
4. potassium of carrying from high sodium polyhalite according to claim 1 and 2 is except the technique of sodium, and it is characterized in that: in step (2), described anionic collector is alkylsulfonate or alkyl sulfate, and its alkyl carbon chain lengths is 10-16.
5. potassium of carrying from high sodium polyhalite according to claim 1 and 2 is except the technique of sodium, it is characterized in that: in step (3), and washing used medium is the mixed liquor of flotation mother liquor and water.
6. potassium of carrying from high sodium polyhalite according to claim 5 is except the technique of sodium, it is characterized in that: the mass ratio of flotation concentrate, flotation mother liquor and water is 10:8-10:1.5-2.0.
CN201510342985.0A 2015-06-19 2015-06-19 Technology for extracting potassium and removing sodium from high-sodium polyhalite ore Pending CN104998748A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN106380233A (en) * 2016-08-29 2017-02-08 化工部长沙设计研究院 Process for preparing potassic-magnesian fertilizer by using polyhalite
CN108714481A (en) * 2018-05-22 2018-10-30 中国科学院青海盐湖研究所 The method that polyhalite is extracted from the polyhalite containing gangue mineral

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106380233A (en) * 2016-08-29 2017-02-08 化工部长沙设计研究院 Process for preparing potassic-magnesian fertilizer by using polyhalite
CN108714481A (en) * 2018-05-22 2018-10-30 中国科学院青海盐湖研究所 The method that polyhalite is extracted from the polyhalite containing gangue mineral
CN108714481B (en) * 2018-05-22 2019-12-13 中国科学院青海盐湖研究所 method for extracting polyhalite from polyhalite ore containing gangue minerals

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