CN104628017A - Method for preparing kainite ore from sulfate-type brine - Google Patents

Method for preparing kainite ore from sulfate-type brine Download PDF

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Publication number
CN104628017A
CN104628017A CN201510079608.2A CN201510079608A CN104628017A CN 104628017 A CN104628017 A CN 104628017A CN 201510079608 A CN201510079608 A CN 201510079608A CN 104628017 A CN104628017 A CN 104628017A
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China
Prior art keywords
kainite
bittern
potassium
saturated
solid
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CN201510079608.2A
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Chinese (zh)
Inventor
张志宏
安东
胡天琦
董生发
马艳芳
张永明
赵冬梅
王婧
付振海
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Qinghai Institute of Salt Lakes Research of CAS
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Qinghai Institute of Salt Lakes Research of CAS
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/133Renewable energy sources, e.g. sunlight

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Abstract

The invention discloses a method for preparing a kainite ore from sulfate-type salt lake brine. The method comprises the following steps of (1) preparing saturated brine of a potassium salt, wherein the saturated brine of the potassium salt contains 2.30-3.50wt% of potassium ions and 4.50-6.50wt% of magnesium ions; (2) carrying out isothermal evaporation on the saturated brine of the potassium salt until a solid is separated out to obtain a solid-liquid mixture; and (3) separating the solid-liquid mixture, wherein the solid phase is the kainite ore, and the liquid phase is a saturated mother solution of the kainite ore. The sulfate-type salt lake brine used in the method is rich in resource, so that the method is suitable for large-scale salt pan production; the energy used in the sunlight evaporation process is solar energy, so that the production cost is low; and the method is simple in operation process and free of dangers. The mother solution obtained by solid-liquid separation can be recycled, so that the potassium resource is sufficiently utilized. Meanwhile, the environment cannot be polluted by using the method, and the obtained product is high in yield, good in quality and environment-friendly.

Description

A kind of vitriolate type bittern prepares the method in kainite ore deposit
Technical field
The invention belongs to Salt Lake Chemistry field, be specifically related to a kind of method that vitriolate type bittern prepares kainite ore deposit.
Background technology
Potassium sulfate is that China is badly in need of and chlorideless potassic fertilizer in short supply for a long time, is again the important source material of production composite fertilizer.The method of producing potassium sulfate at present is both at home and abroad a lot, mainly comprises Mannheim proeess, mirabilite method, gypsum, ammonium sulfate double decomposition, forms the method for putting, solvent extration and ion exchange method etc.From the existing resource distribution situation of China, the area such as Qinghai, Xinjiang, Tibet has abundant salt lake brine resource, this resource is utilize salt lake brine to produce potassium sulfate to provide sufficient raw material, the method utilizing salt lake brine to produce potassium sulfate is with sun power Exposure to Sunlight concentrated brine, kainite is separated out in further evaporation, kainite is transported into factory process and becomes schoenite, adds Repone K metathesis and changes into potassium sulfate., as the intermediates producing potassium sulfate, there is important effect in kainite ore deposit in potassium sulfate production process.Produce due to solar evaporation and belong to extensive property technology, the Quality and yield in kainite ore deposit is very large by the impact of production technique and natural cause, the fluctuation of mineral quality causes very adverse influence to the production of subsequent sulphuric acid potassium, and therefore production higher-grade, high quality kainite ore deposit are very urgent.
Patent documentation CN103738983A discloses a kind of use prepares kainite technique containing the thick product of potassium seven water epsom salt, comprise the following steps: (1) by containing the thick product of potassium seven water epsom salt with to the saturated epsom salt mother liquor of magnesium sulfate or old halogen in mass ratio 1:1-3 convert halogen, then add in thermosol groove and be heated to 60-90 DEG C, 0.5-4 hour is dissolved in insulation, obtains hot halogen; (2) hot for step (1) gained halogen insulation filtered, filter residue is thick kainite; (3) the thick kainite of step (2) gained is added the water plasm scouring being again equivalent to thick kainite weight 1-4 times, obtain high-quality kainite and wash and starch water again containing potassium; (4) step (3) gained is washed and starched water again containing potassium and return step (1), replace epsom salt mother liquor used or old halogen in step (1) to use.But there is complex technical process, the more high defect of energy consumption in this application.
Summary of the invention
For preparing the shortcomings such as kainite ore deposit grade is low, of poor quality in prior art, the invention provides that a kind of energy consumption is low, efficiency is high, be applicable to the preparation method in scale operation kainite ore deposit, salt pan.
The invention provides a kind of method that sulfate type salt lake brine prepares kainite ore deposit, comprise the following steps:
(1) prepare sylvite saturated bittern, potassium content 2.30wt% ~ 3.50wt% in described sylvite saturated bittern, magnesium ion content 4.50wt% ~ 6.50wt%, it obtains by converting the approach such as halogen or evaporation.
(2) carrying out isothermal evaporation to described sylvite saturated bittern to separate out to there being solid, obtaining solidliquid mixture.
Preferably, step 2) described in isothermal evaporation process lasts to saturated bittern there is following composition: potassium content is 0.80wt% ~ 1.5wt%, and magnesium ion content is 7.00wt% ~ 8.00wt%.
Preferably, described isothermal evaporation temperature is 27-33 degree Celsius, relative air humidity: 12% ~ 20%.
(3) be separated by above-mentioned solidliquid mixture, wherein, solid phase is kainite ore deposit, and liquid phase is the saturated mother liquor of kainite.
Preferably, the saturated mother liquor of described kainite is used for the preparation of sylvite saturated bittern in step (1).
The present invention has the following advantages:
1, the vitriolate type bittern aboundresources that the present invention is used, is applicable to large-scale Solar pond production;
2, the solar evaporation process energy used is sun power, and production cost is low;
3, operating process of the present invention is simple, without dangerous.For the mother liquor that solid-liquid separation obtains, recyclable recirculation uses, and takes full advantage of potassium resource.The method environmentally safe simultaneously, the product obtained, productive rate is high, and quality is good, environmental protection.
Accompanying drawing explanation
Fig. 1, process flow sheet of the present invention.
The XRD figure of the product that Fig. 2, the present invention obtain.
Embodiment
Embodiment 1:
The present embodiment comprises the following steps:
(1) carry out solar evaporation until sylvite is saturated to the vitriolate type bittern of field acquisition, then regulate this bittern composition by converting halogen mode, after making adjustment, bittern consists of potassium content 2.61wt%, magnesium ion content 6.02wt%;
(2) take step (1) gained bittern 964.6g, be placed in rigid plastics evaporator tank, be placed in evaporation at constant temperature room and carry out isothermal evaporation.Control brine temperature: 27 ± 0.5 DEG C, relative air humidity: 12% ~ 20%;
(3) moisture weight lost when bittern evaporation in step (2) is 201.2g, potassium content 0.84wt% in liquid phase, during magnesium ion content 7.78wt%, is separated, obtains solid sample 238.7g to evaporation gained solidliquid mixture;
(4) carry out XRD test (as shown in Figure 2) to the solid sample obtained in step (3), determine that obtaining solid sample is kainite ore deposit, wherein kainite content is 80.7%, and liquid phase converts halogen for step 1.
Embodiment 2:
The present embodiment comprises the following steps:
(1) carry out solar evaporation until sylvite is saturated to the vitriolate type bittern of field acquisition, then regulate this bittern composition by converting halogen mode, after making adjustment, bittern consists of potassium content 3.13wt%, magnesium ion content 5.12wt%;
(2) take step (1) gained bittern 1124.8g, be placed in rigid plastics evaporator tank, be placed in evaporation at constant temperature room and carry out isothermal evaporation.Control brine temperature: 27 ± 0.5 DEG C, relative air humidity: 12% ~ 20%;
(3) moisture weight lost when bittern evaporation in step (2) is 276.4g, potassium content 1.55wt% in liquid phase, during magnesium ion content 7.31wt%, is separated, obtains solid sample 226.4g to evaporation gained solidliquid mixture;
(4) carry out XRD test to the solid sample obtained in step (3), determine that obtaining solid sample is kainite ore deposit, wherein kainite content is 73.4%.
Embodiment 3:
The present embodiment comprises the following steps:
(1) carry out solar evaporation until sylvite is saturated to the vitriolate type bittern of field acquisition, then regulate this bittern composition by converting halogen mode, after making adjustment, bittern consists of potassium content 2.36wt%, magnesium ion content 6.24wt%;
(2) take step (1) gained bittern 1044.7g, be placed in rigid plastics evaporator tank, be placed in evaporation at constant temperature room and carry out isothermal evaporation.Control brine temperature: 29 ± 0.5 DEG C, relative air humidity: 12% ~ 20%;
(3) moisture weight lost when bittern evaporation in step (2) is 176.3g, potassium content 1.41wt% in liquid phase, during magnesium ion content 7.35wt%, is separated, obtains solid sample 139.9g to evaporation gained solidliquid mixture;
(4) carry out XRD test to the solid sample obtained in step (3), determine that obtaining solid sample is kainite ore deposit, wherein kainite content is 78.9%.
Embodiment 4:
The present embodiment comprises the following steps:
(1) carry out solar evaporation until sylvite is saturated to the vitriolate type bittern of field acquisition, then regulate this bittern composition by converting halogen mode, after making adjustment, bittern consists of potassium content 2.49wt%, magnesium ion content 5.19wt%;
(2) take step (1) gained bittern 1071.5g, be placed in rigid plastics evaporator tank, be placed in evaporation at constant temperature room and carry out isothermal evaporation.Control brine temperature: 29 ± 0.5 DEG C, relative air humidity: 12% ~ 20%;
(3) moisture weight lost when bittern evaporation in step (2) is 253.9g, potassium content 1.18wt% in liquid phase, during magnesium ion content 6.95wt%, is separated, obtains solid sample 222.8g to evaporation gained solidliquid mixture;
(4) carry out XRD test to the solid sample obtained in step (3), determine that obtaining solid sample is kainite ore deposit, wherein kainite content is 82.3%.
Embodiment 5:
The present embodiment comprises the following steps:
(1) carry out solar evaporation until sylvite is saturated to the vitriolate type bittern of field acquisition, then regulate this bittern composition by converting halogen mode, after making adjustment, bittern consists of potassium content 3.37wt%, magnesium ion content 4.92wt%;
(2) take step (1) gained bittern 1103.8g, be placed in rigid plastics evaporator tank, be placed in evaporation at constant temperature room and carry out isothermal evaporation.Control brine temperature: 33 ± 0.5 DEG C, relative air humidity: 12% ~ 20%;
(3) moisture weight lost when bittern evaporation in step (2) is 229.4g, potassium content 1.24wt% in liquid phase, during magnesium ion content 6.73wt%, is separated, obtains solid sample 190.8g to evaporation gained solidliquid mixture;
(4) carry out XRD test to the solid sample obtained in step (3), determine that obtaining solid sample is kainite ore deposit, wherein kainite content is 83.1%.

Claims (4)

1. prepare the method in kainite ore deposit by sulfate type salt lake brine, comprise the following steps:
(1) sylvite saturated bittern is prepared, potassium content 2.30wt% ~ 3.50wt% in described sylvite saturated bittern, magnesium ion content 4.50wt% ~ 6.50wt%;
(2) carrying out isothermal evaporation to described sylvite saturated bittern to separate out to there being solid, obtaining solidliquid mixture;
(3) be separated by above-mentioned solidliquid mixture, wherein, solid phase is kainite ore deposit, and liquid phase is the saturated mother liquor of kainite.
2. method according to claim 1, is characterized in that, step 2) described in isothermal evaporation process lasts to saturated bittern there is following composition: potassium content is 0.80wt% ~ 1.50wt%, and magnesium ion content is 7.00wt% ~ 8.00wt%.
3. method according to claim 1 and 2, is characterized in that, described isothermal evaporation temperature is 27-33 degree Celsius, relative air humidity: 12% ~ 20%.
4. method according to claim 1 and 2, is characterized in that, the saturated mother liquor of described kainite is used for the preparation of sylvite saturated bittern in step (1).
CN201510079608.2A 2015-02-13 2015-02-13 Method for preparing kainite ore from sulfate-type brine Pending CN104628017A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110650807A (en) * 2017-03-20 2020-01-03 德国钾盐集团股份有限公司 Method for treating salt solutions using a multistage separation process and treatment system for this purpose

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3589871A (en) * 1968-06-10 1971-06-29 Great Salt Lake Minerals Method for the production of high-grade kainite
CN1439602A (en) * 2002-09-25 2003-09-03 新疆罗布泊钾盐科技开发有限责任公司 Preparation of potassium sulfate from brine containing potassium magnesium sulfate
CN1886339A (en) * 2003-12-31 2006-12-27 科学与工业研究委员会 Process for recovery of potassium sulphate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3589871A (en) * 1968-06-10 1971-06-29 Great Salt Lake Minerals Method for the production of high-grade kainite
CN1439602A (en) * 2002-09-25 2003-09-03 新疆罗布泊钾盐科技开发有限责任公司 Preparation of potassium sulfate from brine containing potassium magnesium sulfate
CN1886339A (en) * 2003-12-31 2006-12-27 科学与工业研究委员会 Process for recovery of potassium sulphate

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《盐湖科技资料》编辑: ""高品位钾盐镁矾的生产方法"", 《盐湖科技资料》, no. 01, 2 April 1975 (1975-04-02) *
李海民等: ""卤水资源开发利用技术述评"", 《盐湖研究》, vol. 11, no. 3, 30 September 2008 (2008-09-30), pages 51 - 64 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110650807A (en) * 2017-03-20 2020-01-03 德国钾盐集团股份有限公司 Method for treating salt solutions using a multistage separation process and treatment system for this purpose

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