CN108069444A - A kind of method of comprehensive utilization of sulfate type bittern - Google Patents
A kind of method of comprehensive utilization of sulfate type bittern Download PDFInfo
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- CN108069444A CN108069444A CN201611004896.6A CN201611004896A CN108069444A CN 108069444 A CN108069444 A CN 108069444A CN 201611004896 A CN201611004896 A CN 201611004896A CN 108069444 A CN108069444 A CN 108069444A
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- concentrated brine
- comprehensive utilization
- proportion
- bittern
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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Abstract
The present invention relates to the technical field of salt lake resources comprehensive utilization, especially a kind of method of comprehensive utilization of intercrystalline bittern includes the following steps：Intercrystalline bittern injection salt pan is freezed, obtains the evaporation raw material that proportion is 1.211~1.228；It will be evaporated in the evaporation raw material injection sodium chloride pond, obtain the first concentrated brine and halite that proportion is 1.278~1.288；It will continue to evaporate in first concentrated brine injection potassium mixed salt pond, obtain the second concentrated brine and potassium ores that proportion is 1.302~1.317；It will continue to evaporate in second concentrated brine injection carnallite pond, obtain old halogen and carnallite that proportion is 1.345~1.359.The present invention makes full use of the natural energy resources such as the cold energy, solar energy, wind energy on resource ground extraction salt lake ore resources and lithium is made to be enriched in liquid phase, of low cost, is prepared on a large scale the raw mineral materials for meeting industrial requirements.
Description
Technical field
It is brilliant from a Li Ping salt lakes especially with natural energy resources the present invention relates to the technical field of salt lake resources comprehensive utilization
Between making from brine for carnallite Sync enrichment lithium method.
Background technology
One of an important factor for potash fertilizer is relation China agricultural safety, the salt lake bittern containing potassium provide resource for potash fertilizer production
It ensures.One Li Ping salt lakes of Qinghai are located at western part of Central Tsaidam Basin salt lake band, mineral resources include Brine resources and
Solid salts resources, wherein solid salt mineral resources include halite, saltcake, gypsum, astrakanite and sylvite, and halite is main
Solid saline minerals；Brine resources are intercrystalline bittern, and preservation is divided into upper and lower two layers, water-bearing layer is thicker, halogen in salt deposit is deposited
Containing salts resources such as K, B, Li, Mg, the hydrochemical type of bittern is magnesium sulfate for Shuifu County.It is estimated that resource is stored up in the salt lake
Amount includes 1680.5 ten thousand t of KCl, 179.65 ten thousand t of LiCl, 91.80 ten thousand t of boron oxide, and belonging to has Important Economic valency in Qinghai Province
The salt lake of value, actual according to Brine resources have vast potential for future development to potassium therein, lithium resource rational exploitation and utilization.
One Li Ping salt lakes are located in Central Tsaidam Basin, belong to arid continental climate area, 4 DEG C of average temperature of the whole year, drop in year
Water shortage 25mm, annual mean ground temperature 3500mm, the sunshine-duration is long, mean wind speed 4m/s, and winter is minimum up to or so half a year
Reachable -25 DEG C or so of temperature.
The solar energy and wind energy resources enriched using Yanhu District is separated the saline crystallization in salt lake bittern in salt
It is widely used in terms of the production of lake salt field.Cold energy resource comprehensively utilizes solar energy, the wind of Yanhu District up for developing
Carnallite can be prepared from magnesium sulfate salt lake bittern with cold energy and the lithium in bittern is made to obtain enrichment should have wide hair
Exhibition prospect.
The content of the invention
The method of comprehensive utilization of an inner level ground intercrystalline bittern provided by the invention includes：
1) one li of level ground intercrystalline bittern injection salt pan is freezed, obtains evaporation raw material.
Preferably, the bittern proportion that an inner level ground intercrystalline bittern injection salt pan is refrigerated to reaches 1.211~1.228
When, obtained bittern is as evaporation raw material.
Preferably, the evaporation raw material has following composition Na+78.8~81.7g/L, K+11.4~12.6g/L, Mg2+
23.5~24.7g/L, Cl-185.3~189.1g/L, SO4 2-20.3~24.9g/L, Li+0.24~0.3g/L.
The process in resource winter-spring season can carry out or provide similar environment to carry out refrigerating process.It is described cold
Jelly process should be carried out until bittern is with specific composition or with specific density, and sulfuric acid can be obtained during being somebody's turn to do
The hydrate (saltcake) of sodium.
2) evaporation raw material in summer injection sodium chloride pond is evaporated and separation of solid and liquid, obtained solid phase is sodium chloride,
Obtained bittern is the first concentrated brine.
Preferably, when raw material proportion to be evaporated reaches 1.278~1.288, bittern is separated with solid phase.
Preferably, first concentrated brine has following composition Na+22.1~29.8g/L, K+28.4~31.6g/L,
Mg2+57.7~65.9g/L, Cl-197.9~212.4g/L, SO4 2-55.0~61.5g/L.
3) the first concentrated brine that sodium chloride pond is isolated introduced into potassium mixed salt pond continue evaporation and obtain solid, after by bittern
It is separated with solid phase, obtained solid phase is that (mixture of halite, sylvite and epsomite has a small amount of potassium ores sometimes
Kainite and carnallite), obtained bittern is the second concentrated brine.
Preferably, separation of solid and liquid is carried out when bittern proportion reaches 1.302~1.317.
Preferably, second concentrated brine has following composition Na+1.3~6.4g/L, K+14.1~22.0g/L,
Mg2+85.8~91.1g/L, Cl-241.8~249.5g/L, SO4 2-40.3~61.0g/L.
Preferably, the process can in resource summer and autumn carry out or provide similar environment to be evaporated
Journey.
4) the second concentrated brine is introduced carnallite pond to continue to evaporate, after bittern is separated with solid phase, gained solid phase forms
For halite, hexahydrite and carnallite, obtained bittern is old halogen.
Preferably, separation of solid and liquid is carried out when the second concentrated brine proportion reaches 1.345~1.359.
Preferably, the old halogen has following composition Na+0.5~2.6g/L, K+0.5~1.5g/L, Mg2+110.6~
118.0g/L、Cl-298.2~312.2g/L, SO4 2-40.0~50.9g/L, Li+1.8~2.0g/L.Compared in initial feed
Lithium concentration, concentration improves 5-6 times.
By as above the step of, saltcake, potassium mixed salt, carnallite and old halogen, old halogen can be respectively obtained from intercrystalline bittern
In lithium ion content greatly improved compared with original intercrystalline bittern, can as extraction lithium raw material.
The solid mixture that this step obtains can be separated by way of controlling and being precipitated, and be more segregative
Component can also obtain the tool value product such as potassium chloride by subsequent processing.
Advantageous effect：
Magnesium sulfate salt lake bittern is handled with the method for the present invention, the resources such as potassium therein, magnesium, sulphur is made to obtain rationally
It utilizes, obtained potassium ores and carnallite can be respectively as production potash magnesium sulphate fertilizers and the raw material of potassium chloride, and old halogen can
Raw material as extraction lithium.
The present invention is a kind of technology of environmental protection, and the cold of resource ground is made full use of under the conditions of any chemical reagents are added without
The natural energy resources such as energy, solar energy, wind energy are realized and the industry such as potassium ores, carnallite are obtained from magnesium sulfate salt lake bittern
Potassium-bearing mineral, while lithium is made to be enriched in liquid phase, artificial pollution will not be caused to resource-area, in terms of exploit resources of salt lakes
Have wide practical use.
The method of the present invention implementation cost is cheap, easy to operate, workable, fidelity factor is high, can be prepared on a large scale symbol
Close the raw mineral materials of industrial requirements.
Specific embodiment
It elaborates below to the embodiment of the present invention.
The present invention provides a kind of method of comprehensive utilization of intercrystalline bittern, and solar energy can be utilized to be enriched with and obtain in bittern
Mineral resources.The present embodiment introduces its method of comprehensive utilization by taking one Li Ping salt lakes intercrystalline bittern of the Caidamu Basin as an example.Through analysis
It understands, an inner level ground salt lake bittern belongs to sulfate type, and intercrystalline bittern key component includes：Na+88~94g/L, K+8~9g/L,
Mg2+17~18g/L, Cl-170~175g/L, SO4 2-37~40g/L, Li+0.24~0.3g/L.It is of course also possible to pass through other
Bittern mixes or allotment obtains the bittern of said components to replace intercrystalline bittern.By the intercrystalline bittern introduce specific salt pond,
The potassium-bearing mineral such as carnallite, potassium mixed salt can be prepared after heating evaporation moisture or even prepares raw material as lithium salts.
The method of comprehensive utilization specific steps of one Li Ping salt lakes intercrystalline bittern include：
Step 1 evaporates the acquisition of raw material.
One Li Ping salt lakes intercrystalline bittern injection salt Tanaka is subjected to freezing and obtains evaporation raw material.The proportion of the evaporation raw material
(also known as relative density) is 1.211~1.228, including following component：Na+78.8~81.7g/L, K+11.4~12.6g/
L、Mg2+23.5~24.7g/L, Cl-185.3~189.1g/L, SO4 2-20.3~24.9g/L, Li+0.24~0.3g/L.Wherein,
In order to ensure preparation process optimizes, in evaporation process is monitored on the proportion parameter basis of bittern, potassium ion and sulfuric acid are monitored
Ion concentration is preferred in suitable scope, preferably K+11.4~12.6g/L, SO4 2-20.3~24.9g/L.
Above-mentioned evaporation process can make full use of Caidamu Basin local climate condition to carry out.Usually, after injecting salt pan
Intercrystalline bittern need to freeze, the temperature of freezing is preferably 0 DEG C~-20 DEG C.The Qaidam that average temperature of the whole year is 4 DEG C can be utilized
Basin weather, especially resource winter-spring season or like environment temperature when being less than 0 DEG C outdoor elements can meet freezing
It is required that.The entire refrigerating process should be carried out until bittern is with specific composition or with specific proportion.The crystalline substance
Between brine freezing can obtain the hydrate (saltcake) of sodium sulphate.
Step 2, the acquisition of the first concentrated brine and sodium chloride.
By the evaporation raw material in summer injection sodium chloride pond, evaporated at 10 DEG C~30 DEG C of temperature, treat that proportion reaches
Separation of solid and liquid is carried out when 1.278~1.288, obtained solid phase is sodium chloride, obtains liquid phase as the first concentrated brine.
The component of first concentrated brine includes：Na+22.1~29.8g/L, K+28.4~31.6g/L, Mg2+57.7~
65.9g/L、Cl-197.9~212.4g/L, SO4 2-55.0~61.5g/L.Wherein, in order to ensure preparation process optimizes, supervising
It controls in evaporation process on the proportion parameter basis of bittern, monitors potassium ion and sulfate ion concentration is in suitable scope
It is good, preferably K+28.4~31.6g/L, SO4 2-58.3~60.7g/L.
The process can be during temperature range is 10 DEG C~30 DEG C, such as summer carries out.
Step 3, the acquisition of the second concentrated brine and potassium mixed salt.
First concentrated brine is introduced potassium mixed salt pond to be evaporated, when liquid phase proportion reaches 1.302~1.317 into
Row separation of solid and liquid, obtained solid phase are potassium mixed salt, and obtained bittern is the second concentrated brine.Usually, people in the art
Member understands that the component of potassium mixed salt includes：Halite (chemical composition is sodium chloride), sylvite (chemical composition is potassium chloride) and rush down profit
Salt (chemical composition is epsom salt) and have a small amount of kainite and carnallite sometimes).
Wherein, the component of second concentrated brine includes：Na+1.3~6.4g/L, K+14.1~22.0g/L, Mg2+
85.8~91.1g/L, Cl-241.8~249.5g/L, SO4 2-40.3~61.0g/L.In order to ensure preparation process optimizes,
It monitors in evaporation process on the proportion parameter basis of bittern, monitors potassium ion and sulfate ion concentration is in suitable scope
It is good, preferably K+14.1~22.0g/L, SO4 2-40.3~61.0g/L.
Step 4：The acquisition of carnallite and old halogen
Through second concentrated brine carnallite pond is introduced to be evaporated, when liquid phase proportion reaches 1.345~1.359 into
Row separation of solid and liquid, can obtain carnallite and old halogen, and the mineral composition of carnallite is halite, hexahydrite and carnallite, always
Halogen composition is Na+0.5~2.6g/L, K+0.5~1.5g/L, Mg2+110.6~118.0g/L, Cl-298.2~312.2g/L,
SO4 2-40.0~50.9g/L, Li+1.8~2.0g/L.Compared with the lithium concentration in initial feed, concentration improves 5-6
Times.
In conclusion the method provided by the invention to intercrystalline bittern comprehensive utilization can be by providing by natural energy resources
Any chemical reagents are not added the potassium-bearing minerals such as carnallite, potassium ores are prepared, while lithium is made to obtain richness in liquid phase in source
Collection, will not cause resource-area artificial pollution, have wide practical use in terms of exploit resources of salt lakes.
The above is the specific embodiment of the present invention, the citing that its purpose is to clearly illustrate the present invention and make,
It is not the restriction to embodiments of the present invention.For those of ordinary skill in the art, in the base of above description
It can also be made other variations or changes in different ways on plinth.There is no need and unable to give thoroughly all embodiments
It lifts.All any modification, equivalent and improvement made within the spirit and principles of the invention etc., should be included in the present invention
Within scope of the claims.
Claims (8)
1. a kind of method of comprehensive utilization of sulfate type bittern, which is characterized in that include the following steps：
Evaporate the acquisition of raw material：Intercrystalline bittern injection salt pan is freezed in winter；At a temperature of winter environment, after separation of solid and liquid
Obtain the evaporation raw material that proportion is 1.211~1.228；
The acquisition of first concentrated brine：By the evaporation raw material in summer injection sodium chloride pond, evaporated at a temperature of summer environment,
Separation of solid and liquid, which is carried out, when the evaporation raw material proportion is 1.278~1.288 obtains the first concentrated brine and sodium chloride；
The acquisition of second concentrated brine and potassium mixed salt：Potassium mixed salt is injected at a temperature of summer environment, by first concentrated brine
Continue to evaporate in pond, carrying out separation of solid and liquid when proportion is 1.302~1.317 obtains the second concentrated brine and potassium ores.
The acquisition of carnallite：It at a temperature of summer environment, will continue to evaporate in second concentrated brine injection carnallite pond, treat
Carnallite and old halogen, wherein Li are obtained when bittern proportion is 1.345~1.359 after separation of solid and liquid+Concentration is 1.8~2.0g/
L。
2. the method for comprehensive utilization of sulfate type bittern according to claim 1, which is characterized in that the evaporation raw material components
Including：Na+78.8~81.7g/L, K+11.4~12.6g/L, Mg2+23.5~24.7g/L, Cl-185.3~189.1g/L, SO4 2-
20.3~24.9g/L, Li+0.24~0.3g/L.
3. the method for comprehensive utilization of sulfate type bittern according to claim 1, which is characterized in that first concentrated brine
Component include：Na+22.1~29.8g/L, K+28.4~31.6g/L, Mg2+57.7~65.9g/L, Cl-197.9~212.4g/
L、SO4 2-55.0~61.5g/L.
4. the method for comprehensive utilization of sulfate type bittern according to claim 3, which is characterized in that first concentrated brine
In, SO4 2-Concentration is 58.3~60.7g/L.
5. the method for comprehensive utilization of sulfate type bittern according to claim 1, which is characterized in that second concentrated brine
Component include：Na+1.3~6.4g/L, K+14.1~22.0g/L, Mg2+85.8~91.1g/L, Cl-241.8~249.5g/L,
SO4 2-40.3~61.0g/L.
6. the method for comprehensive utilization of sulfate type bittern according to claim 1, which is characterized in that the component bag of the old halogen
It includes：Na+0.5~2.6g/L, K+0.5~1.5g/L, Mg2+110.6~118.0g/L, Cl-298.2~312.2g/L, SO4 2-40.0
~50.9g/L.
7. the method for comprehensive utilization of sulfate type bittern according to claim 6, which is characterized in that in the old halogen, K+Concentration
0.5~1.0g/L, SO4 2-40.3~49.3g/L of concentration.
8. the method for comprehensive utilization of sulfate type bittern according to claim 1, which is characterized in that the winter environment temperature
Scope is -20 DEG C~0 DEG C；The summer environment temperature range is 10 DEG C~30 DEG C.
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| CN201611004896.6A CN108069444A (en) | 2016-11-15 | 2016-11-15 | A kind of method of comprehensive utilization of sulfate type bittern |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109292801A (en) * | 2018-12-05 | 2019-02-01 | 中国科学院青海盐湖研究所 | A kind of preparation method of food-grade magnesium chloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910652A (en) * | 2012-10-18 | 2013-02-06 | 中国科学院青海盐湖研究所 | Clean production process of plateau sulfate type boron-lithium salt lake brine |
-
2016
- 2016-11-15 CN CN201611004896.6A patent/CN108069444A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910652A (en) * | 2012-10-18 | 2013-02-06 | 中国科学院青海盐湖研究所 | Clean production process of plateau sulfate type boron-lithium salt lake brine |
| CN103204520A (en) * | 2012-10-18 | 2013-07-17 | 中国科学院青海盐湖研究所 | Method for preparing single-form potassic salt ore from plateau sulfate type salt lake brine |
| CN103204523A (en) * | 2012-10-18 | 2013-07-17 | 中国科学院青海盐湖研究所 | Method for preparing lithium salt ore from plateau sulfate type salt lake brine |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109292801A (en) * | 2018-12-05 | 2019-02-01 | 中国科学院青海盐湖研究所 | A kind of preparation method of food-grade magnesium chloride |
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