CN108149321A - A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake - Google Patents
A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake Download PDFInfo
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- CN108149321A CN108149321A CN201711424736.1A CN201711424736A CN108149321A CN 108149321 A CN108149321 A CN 108149321A CN 201711424736 A CN201711424736 A CN 201711424736A CN 108149321 A CN108149321 A CN 108149321A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of methods of bittern production basic magnesium carbonate whisker for recycling dried-up lake.This method includes the following steps：By bittern and water in mass ratio 1：After 1.3~1.8 are mixed dissolving in salt pond, brine is filtered to obtain；The Na of 0.9~1.1 mol/L is added in into brine2CO3Solution filters after natural evaporation concentrates, obtains filtrate and precipitation, precipitation is washed, dry after obtain basic magnesium carbonate whisker；The brine and the Na2CO3Volume ratio be 1：1.2~1.6；Filtrate is subjected to natural evaporation concentration, makes magnesium ion concentration after 2.1~3.1 mol/L, to discard insoluble matter, rejoining Na2CO3Solution, into cycle production next time.Up to 12 times, the purity of basic magnesium carbonate whisker realizes the high-value-use of resource up to 95%~98% for present invention cycle production.
Description
Technical field
The invention belongs to inorganic materials technical field, more particularly, to a kind of salt for recycling dried-up lake
The method that halogen produces basic magnesium carbonate whisker.
Background technology
China possesses abundant liquid magnesium resource, and geological mapping report shows that only Qinghai Salt Lake magnesium chloride reserves are just up to hundred million
Ton, hundred million tons of magnesium sulfate, account for more than the 87% of national magnesium salts reserves.Dried-up lake is referred to due to long-term wind, solarization and strong
Evaporation so that salt lake is in dry or half dry state, and the soil just ploughed just as tractor of looking far into the distance is the same.It is dry
Bittern in salt lake refers to that High Concentration Brine is condensed into the salt block of solid block after drying out, contains in this bittern
There are the inorganic salts such as abundant magnesium chloride, sodium chloride, only one ground of Qinghai Cha Er Han, every year because KCl production discharge chlorination magnesium amount is high
Up to ten thousand tons, formed " magnesium evil ".But major part magnesium carbonate in China's prepares raw material and is but mainly derived from solid more than impurity at present
Ore deposit, product quality are difficult to improve, and fine type carbonic acid magnesium products quantitatively or in quality cannot meet the market demand.
Industrial widely applied magnesium carbonate is basic magnesium carbonate at present.Since basic magnesium carbonate is unformed secondary group
Poly- particle has larger specific surface area, and the impurity of adsorption is more, and its mechanical property is poor, as composite material
Among filler is for rubber, plastics, the mechanical property of basis material can be reduced to some extent.Magnesium carbonate whisker is magnesium carbonate
Monocrystal, molecular formula MgCO3·nH2O, wherein n=1~5.Compared with common basic magnesium carbonate, magnesium carbonate whisker is brilliant
The defects of body is not only developed completely, whisker water white transparency, and crystal includes is few, impurity is few, crystal intensity is high, shows pole
Good physics, chemical property and excellent mechanical property, can be directly used for such as rubber, paint, papermaking, medical product, makeup
The fields such as product, construction material and ceramic material.
The crystallization process of basic magnesium carbonate whisker is very sensitive, is mixed, addition, system pH, alkali concn, reacts temperature
The regulation and control of many factors such as degree, reaction time and additive influence.Since the complexity of magnesium carbonate preparation system so that magnesium carbonate is brilliant
The research of palpus mechanism is complex, and the preparation of magnesium carbonate whisker predominantly stays in the exploratory experiment stage at present, and China is not carried out
The production of industrialized level.And at present mainly using chemical reagent, solid magnesium ore deposit as raw material, directly by the use of liquid magnesium as react
The research of raw material is less, and using liquid magnesium as the preparation method of raw material, it needs to add in aqueous alkali, strong acid liquid or oxidant etc.,
After extracting a whisker, the physico-chemical attributes of brine become more complicated, and the trace element enrichment speed in brine can become very slow,
So that magnesium chloride easily reaches saturation, even if injecting lye into system again at this time, new cycle can not be formed, thus cannot
Play salt lake and liquid magnesium resource advantage.In addition, aqueous alkali, strong acid liquid or oxidant for adding in etc. be easy to cause metal instrumentation corruption
Erosion and glass apparatus crush, harsher to requirements such as reaction temperature and reaction time, are unfavorable for industrialized production.
Therefore, how the basic magnesium carbonate crystal whisker products for high added value being converted into just as the magnesium chloride of chicken ribs, change give up into
Treasured for pushing Western Economic, optimizing the structure of production, promotes magnesium resource comprehensive utilization in salt lake to have positive effect.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies of existing basic magnesium carbonate crystal whisker preparation method, provide one kind
The method for recycling the bittern production basic magnesium carbonate whisker of dried-up lake.The method of the present invention is to originate from the bittern of dried-up lake
For raw material, by allocating the whisker required condition of growth straight, using the self-cleaning of whisker, cycle is produced with whisker morphology
Functionalization carbonic acid magnesium material changes the defective mode that the bittern of dried-up lake leaves unused always, solves metal instrumentation easily quilt
The problems such as burn into glass apparatus is broken realizes resource high-value-use.
It is brilliant that first of the present invention is designed to provide a kind of bittern production basic magnesium carbonate for recycling dried-up lake
The method of palpus.
The basic magnesium carbonate whisker being prepared another object of the present invention is to provide the method.
The above-mentioned purpose of the present invention is achieved by the following technical programs：
A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake, includes the following steps：
S1. by bittern and water in mass ratio 1：After 1.3~1.8 are mixed dissolving in salt pond, brine is filtered to obtain；
S2. the Na of 0.8~1.1mol/L is added in into brine2CO3Solution is filtered after natural evaporation concentrates, is filtered
Liquid and precipitation, precipitation is washed, dry after obtain basic magnesium carbonate whisker；The brine and Na2CO3Volume ratio be 1：
1.2~1.6；
S3. the filtrate is subjected to natural evaporation concentration, makes magnesium ion concentration after 2.1~3.1mol/L, to discard insoluble
Object rejoins Na2CO3Solution, into cycle production next time.
Containing the inorganic salts such as abundant magnesium chloride, sodium chloride in bittern in dried-up lake, by bittern be dissolved in volume compared with
After in big outdoor artificial salt pond, the dosage of water is controlled so that bittern is still within after being dissolved in water or close to high concentration state
(i.e. metastable state, in a state in which dense salt system once precipitating reagent is added in very easily be precipitated crystallization.According to alkali formula can be precipitated
The condition of magnesium sulfate crystal whisker under the conditions of wind or shining upon grade natural evaporations concentration, controls the Na of addition2CO3Dosage,
Basic magnesium carbonate whisker precipitation can be prepared into, reaction equation is as follows：
It is mainly the substances such as water, sodium chloride and other soluble-salts after basic magnesium carbonate whisker is separated by filtration, in filtrate,
At this point, magnesium ion concentration necessarily reduces in filtrate systems.If by precipitation filtrates continue natural evaporation concentration, sodium chloride and some
The smaller salt of solubility is then precipitated due to the reduction of solvent, but since the solubility because of magnesium chloride is larger, thus magnesium chloride this
Shi Buhui is precipitated, therefore the concentration of magnesium chloride inevitably enlarges.The growth of lucky basic magnesium carbonate whisker requires magnesium chloride to have centainly
Concentration, at this moment if injecting Na into precipitation filtrates again2CO3, you can the cycle into a new round produces.
Preferably, the number of the cycle production is up to 12 times；The purity of basic magnesium carbonate whisker being prepared >=
95%.Sodium chloride, potassium chloride and some other salt can be precipitated, and water can be distilled out of, but still have fraction component such as iron ion,
Aluminium ion etc., still stays in system, and with increasing for cycle-index, the concentration accumulation of these components is increasing, as a result makes
It obtains basic magnesium carbonate crystal whisker products and receives contamination, cause the reduction of whisker purity, do not meet national standard.The present invention is by a large amount of
Research and explorative experiment prove, in the dense salt system in above-mentioned salt pond, basic magnesium carbonate whisker recycles the number of production up to 12 times,
Since the 13rd time, it is more than the impurity such as iron and the aluminium of national Specification that basic magnesium carbonate crystal whisker products, which start contamination to have content,.
" self-cleaning " of whisker refer to whisker atomic arrangement high-sequential, intact filling or seldom lack filling, difficult adsorbing contaminant,
The characteristic that difficulty is infected with by impurity.Its scientific basis is：First, whisker is free of or seldom containing defective；Second, the whisker surface field of force
In high degree of symmetry distribution and specific surface area it is small, thus be not easy adsorbing contaminant, according to surface chemistry theory, the surface field of force is more symmetrical,
Specific surface area is smaller, just smaller to the adsorption capacity of impurity, is more difficult to that chemisorbed occurs；Third, whisker will in growth course
It asks growth unit that must have specific stabilization energy, otherwise cannot enter lattice, only exist physical absorption, this weak object at this time
Reason absorption only need to be washed with water and can remove the impurity of absorption.But whisker grow straight play its self-cleaning be to have ready conditions
, it is not that adsorbing contaminant or can be infected in no instance by impurity.What this condition referred to is exactly whisker growth system
Suitable Chemical Physics condition, such as the concentration of alkali and addition, system pH, reaction temperature, reaction time.
The present invention mainly using under certain preparation condition, basic magnesium carbonate whisker have in itself be not easy to be infected with,
It is not easy absorption and carries " self-cleaning " characteristic of impurity secretly so that the preparation process of basic magnesium carbonate whisker avoids complicated removal of impurities
Process directly prepares whisker without purification ＆ isolation with bittern, by controlling Na in each round cycle production2CO3The concentration of solution with
Addition, the concentration of magnesium ion, evaporation time, evaporation rate and evaporating temperature etc., cycle production, which obtains constructor synthetic, to produce
Product standard, whisker draw ratio may be up to 20：1, the basic magnesium carbonate crystal whisker products of purity >=95%.
Preferably, the Na2CO3A concentration of 0.90~1.10mol/L of solution.
Preferably, the magnesium ion concentration described in step S3 is 2.1~3.1mol/L.
Preferably, the time of the natural evaporation is 3~5d, and mean temperature is 20~25 DEG C (preferably 23 DEG C).According to dry
Dry up the bittern system compositing characteristic in salt lake, selects the Na of various concentration2CO3Solution, magnesium ion and different evaporation rates are come
Prepare basic magnesium carbonate whisker.
Preferably, described to be filtered into filtered through gauze, suction filtration, micro-filtration, nanofiltration or ultrafiltration, precipitation filtrates can be recycled.
Preferably, the washing is washing 4~6 times.
Preferably, the drying described in step S2 is that microwave drying is carried out at 70~90 DEG C.
Preferably, the leading ion molar concentration in the step S1 in the brine of gained is：Mg2+2.1~3.1mol/L,
Cl-2.4~3.8mol/L, K+0.8~2.2mol/L, Na+0.4~1.3mol/L.
Preferably, the insoluble matter described in the step S3 is sodium chloride and potassium chloride, can carry out resource reutilization.
The present invention also provides the basic magnesium carbonate whisker being prepared using the above method, the basic magnesium carbonate whisker
Whisker draw ratio be 18~20：1, and its purity >=95% (95%~98%).
Compared with prior art, the invention has the advantages that：
The present invention is raw material using the bittern of the impurity containing particular types and quantity in dried-up lake, by adjusting
Na2CO3Solution, the concentration of magnesium ion and a series of indexs such as mixing velocity and evaporation rate control whisker growth system
The basic magnesium carbonate whisker of high-purity is made in condition, and product whisker draw ratio is up to 20 after measured：1, purity >=95%, product
Stable quality；And the filtrate in product precipitation process can recycle, and obtained byproduct sodium chloride and potassium chloride also may be used
Resource reutilization, realizes the high-value-use of salt lake resources and dried-up lake magnesium resource, and the bittern for changing dried-up lake is not busy always
The defective mode put solves the problems such as metal instrumentation is easily corroded, glass apparatus is broken.Present invention process is simply easy
It is capable, pollution-free, at low cost, it can be achieved that large-scale production.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
It is further illustrated the present invention below in conjunction with Figure of description and specific embodiment.Following embodiment for the present invention compared with
Good embodiment, but protection scope of the present invention is not limited in any form.Simply join in embodiment of the present invention
Several replacements cannot in embodiment repeat, but be not intended to limit the present invention one by one, other any without departing from the present invention's
Spirit Essence with made under principle change, modification, replacement, combine, simplification, equivalent substitute mode should be considered as, should all be wrapped
Containing within the scope of the present invention.
Unless stated otherwise, the reagent of the invention used, method and apparatus for the art conventional reagent, method and are set
It is standby.Unless stated otherwise, following embodiment agents useful for same and material are purchased in market.
Embodiment 1
A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake, includes the following steps：
(1) it is 7.5m in volume3Salt pond in, introduce 2 tons of bittern, add in tap water, stir to bittern and all dissolve.
Liquor capacity is measured as 2.8m3, filter, discard insoluble matter, obtain brine；Wherein, the mass ratio of bittern and water is 1：1.3.
(2) Na of 1.0mol/L is added in into brine2CO3Solution 2m3, it is (flat after the natural evaporations such as wind, solarization concentration 4d
Equal temperature is 23 DEG C), with fine and close filtered through gauze brine, filtrate and basic magnesium carbonate whisker precipitation are obtained, by the precipitation with water
Washing 4 times obtains the basic magnesium carbonate crystal whisker products of high-purity after carrying out microwave drying at 80 DEG C；
(3) filtrate obtained by (2) step is placed in sunlight to be exposed to the sun, natural evaporation is dried out, and (process can generate chlorine
Change sodium and potassium chloride precipitation), make magnesium ion concentration after 2.6mol/L, to rejoin Na2CO3Solution, into cycle next time
Production.
This method is recycled production 12 times, and after cycle produces 12 times, the impurity composition concentration in reaction system increases,
At this moment impurity can be infected with whisker, decline whisker purity, therefore can only recycle production 12 times.Basic magnesium carbonate prepared by this method
The yield of whisker is 99%, and whisker draw ratio is 20：1, purity 98%.
Embodiment 2
A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake, includes the following steps：
(1) it is 7.5m in volume3Salt pond in, introduce 2 tons of bittern, add in tap water, stir to bittern and all dissolve.
Liquor capacity is measured as 2.9m3, filter, discard insoluble matter, obtain brine；Wherein, the mass ratio of bittern and water is 1：1.4.
(2) Na of 1.1mol/L is added in into brine2CO3Solution 2m3, it is (flat after the natural evaporations such as wind, solarization concentration 4d
Equal temperature is 24 DEG C), with fine and close filtered through gauze brine, filtrate and basic magnesium carbonate whisker precipitation are obtained, by the precipitation with water
Washing 5 times obtains the basic magnesium carbonate crystal whisker products of high-purity after carrying out microwave drying at 80 DEG C；
(3) filtrate obtained by (2) step is placed in sunlight to be exposed to the sun, natural evaporation is dried out, and (process can generate chlorine
Change sodium and potassium chloride precipitation), make magnesium ion concentration after 2.1mol/L, to rejoin Na2CO3Solution, into cycle next time
Production.
This method is recycled production 12 times, and after cycle produces 12 times, the impurity composition concentration in reaction system increases,
At this moment impurity can be infected with whisker, decline whisker purity, therefore can only recycle production 12 times.Basic magnesium carbonate prepared by this method
The yield of whisker is 98%, and whisker draw ratio is 19：1, purity 97%.
Embodiment 3
A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake, includes the following steps：
(1) it is 7.5m in volume3Salt pond in, introduce 2 tons of bittern, add in tap water, stir to bittern and all dissolve.
Liquor capacity is measured as 2.8m3, filter, discard insoluble matter, obtain brine；Wherein, the mass ratio of bittern and water is 1：1.4.
(2) Na of 1.08mol/L is added in into brine2CO3Solution 2m3, it is (flat after the natural evaporations such as wind, solarization concentration 5d
Equal temperature is 24 DEG C), with fine and close filtered through gauze brine, filtrate and basic magnesium carbonate whisker precipitation are obtained, by the precipitation with water
Washing 5 times obtains the basic magnesium carbonate crystal whisker products of high-purity after carrying out microwave drying at 80 DEG C；
(3) filtrate obtained by (2) step is placed in sunlight to be exposed to the sun, natural evaporation is dried out, and (process can generate chlorine
Change sodium and potassium chloride precipitation), make magnesium ion concentration after 3.1mol/L, to rejoin Na2CO3Solution, into cycle next time
Production.
This method is recycled production 12 times, and after cycle produces 12 times, the impurity composition concentration in reaction system increases,
At this moment impurity can be infected with whisker, decline whisker purity, therefore can only recycle production 12 times.Basic magnesium carbonate prepared by this method
The yield of whisker is 97%, and whisker draw ratio is 18：1, purity 96%.
Embodiment 4
A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake, includes the following steps：
(1) it is 7.5m in volume3Salt pond in, introduce 2 tons of bittern, add in tap water, stir to bittern and all dissolve.
Liquor capacity is measured as 2.9m3, filter, discard insoluble matter, obtain brine；Wherein, the mass ratio of bittern and water is 1：1.5.
(2) Na of 0.98mol/L is added in into brine2CO3Solution 2m3, it is (flat after the natural evaporations such as wind, solarization concentration 4d
Equal temperature is 23 DEG C), with fine and close filtered through gauze brine, filtrate and basic magnesium carbonate whisker precipitation are obtained, by the precipitation with water
Washing 5 times obtains the basic magnesium carbonate crystal whisker products of high-purity after carrying out microwave drying at 90 DEG C；
(3) filtrate obtained by (2) step is placed in sunlight to be exposed to the sun, natural evaporation is dried out, and (process can generate chlorine
Change sodium and potassium chloride precipitation), make magnesium ion concentration after 2.5mol/L, to rejoin Na2CO3Solution, into cycle next time
Production.
This method is recycled production 12 times, and after cycle produces 12 times, the impurity composition concentration in reaction system increases,
At this moment impurity can be infected with whisker, decline whisker purity, therefore can only recycle production 12 times.Basic magnesium carbonate prepared by this method
The yield of whisker is 97%, and whisker draw ratio is 20：1, purity 95%.
Comparative example 1
The method that this comparative example produces basic magnesium carbonate whisker, substantially the same manner as Example 1, difference lies in this comparative examples
Na2CO3The addition of solution is different.Na2CO3The addition of solution is respectively the Na of 0.40mol/L2CO3Solution 2m3With
The Na of 1.0mol/L2CO3Solution 2.5m3。
Experimental result is shown, adds in the Na of 0.40mol/L2CO3Solution 2m3, no whisker generation, because of Na2CO3Amount too
It is low, it is impossible to generation whisker is reacted with magnesium ion；Add in the Na of 1.0mol/L2CO3Solution 2.5m3, Na2CO3Volume it is too big, generation
Whisker contain impurity, purity is only 68%, yield 30%.
Comparative example 2
The method that this comparative example produces basic magnesium carbonate whisker, substantially the same manner as Example 1, difference lies in this comparative example steps
Suddenly the concentration of control magnesium ion is different in (3).The concentration of magnesium ion is adjusted to 1.8mol/L, 3.5mol/ respectively in this comparative example
L。
Experimental result shows, during a concentration of 1.8mol/L of magnesium ion, no whisker generation, because the concentration of magnesium ion is too
It is low, it is impossible to Na2CO3Reaction generation whisker；During a concentration of 3.5mol/L of magnesium ion, with Na2CO3The whisker of reaction generation contains
There is impurity, purity is only 70%, and whisker draw ratio is 16：1, yield 26%.
Comparative example 3
The method that this comparative example produces basic magnesium carbonate whisker, substantially the same manner as Example 1, difference lies in this comparative example steps
Suddenly the condition that natural evaporation concentrates in (2) is different.The condition that natural evaporation concentrates in this comparative example is respectively set to：(1) time
For 7d, mean temperature is 23 DEG C；(2) time is 4d, and mean temperature is respectively 15 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, is had studied
The situation of change of product within the scope of an extensive temperature.
The experimental results showed that the overlong time of processing (1) natural evaporation, the basic magnesium carbonate whisker of generation contain impurity,
Its purity is only 86%, and whisker draw ratio is 15：1, yield 82%.It is 15 DEG C and 30 to handle the mean temperature evaporated in (2)
DEG C when, the diffraction maximum half-peak breadth of the product of acquisition is wider and sample crystallinity is relatively low；When reaction temperature is 25 DEG C, synthesized product
Pattern be whisker, and with relatively narrow half-peak breadth and higher crystallinity；And with the raising of temperature, reaction temperature 35
Compared with other it is then impurity phase occurred at~40 DEG C.
Claims (9)
- A kind of 1. method of bittern production basic magnesium carbonate whisker for recycling dried-up lake, which is characterized in that including following Step：S1. by bittern and water in mass ratio 1：After 1.3~1.8 are mixed dissolving in salt pond, brine is filtered to obtain；S2. the Na of 0.9~1.1 mol/L is added in into brine2CO3Solution filters after natural evaporation concentrates, obtains filtrate And precipitation, precipitation is washed, dry after obtain basic magnesium carbonate whisker；The brine and Na2CO3Volume ratio be 1：1.2 ~1.6；S3. the filtrate is subjected to natural evaporation concentration, makes magnesium ion concentration after 2.1~3.1 mol/L, to discard insoluble matter, Rejoin Na2CO3Solution, into cycle production next time.
- 2. according to the method described in claim 1, it is characterized in that, the number of the cycle production is up to 12 times.
- 3. according to the method described in claim 1, it is characterized in that, the magnesium ion concentration described in step S3 is 2.5~2.7 mol/L。
- 4. according to the method described in claim 1, it is characterized in that, the time of the natural evaporation be 3~5 d, mean temperature It is 20~25 DEG C.
- 5. according to the method described in claim 1, it is characterized in that, the washing is washing 4~6 times.
- 6. according to the method described in claim 1, it is characterized in that, the drying described in step S2 is done at 70~90 DEG C It is dry.
- 7. according to the method described in claim 1, it is characterized in that, leading ion in the step S1 in the brine of gained A concentration of Mg2+2.1~3.1mol/L, Cl-2.4~3.8mol/L, K+0.8~2.2mol/L, Na+0.4~1.3mol/L.
- 8. the basic magnesium carbonate whisker that claim 1~7 any one of them method is prepared.
- 9. basic magnesium carbonate whisker according to claim 8, which is characterized in that the whisker of the basic magnesium carbonate whisker is long Diameter ratio is 18~20：1, and its purity >=95%.
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| CN115676854A (en) * | 2022-09-08 | 2023-02-03 | 西安交通大学 | Method for jointly preparing battery-grade sodium carbonate and basic magnesium carbonate in soda ash industry |
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| 吴健松等: "徐闻盐场苦卤制备Mg2(OH)2CO3•3H2O晶须", 《人工晶体学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115676854A (en) * | 2022-09-08 | 2023-02-03 | 西安交通大学 | Method for jointly preparing battery-grade sodium carbonate and basic magnesium carbonate in soda ash industry |
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Application publication date: 20180612 |