CN108166062A - It is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker - Google Patents
It is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker Download PDFInfo
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- CN108166062A CN108166062A CN201711423193.1A CN201711423193A CN108166062A CN 108166062 A CN108166062 A CN 108166062A CN 201711423193 A CN201711423193 A CN 201711423193A CN 108166062 A CN108166062 A CN 108166062A
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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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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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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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses it is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, include the following steps:S1. it is 77 ~ 83 DEG C brine to be filtered and keep temperature, and Na is then added dropwise into brine under stiring2SO4/ NaOH mixed solutions, mixed system is obtained after dripping;A concentration of 2.3 ~ 3.2mol/L of magnesium ion in the brine, the brine and the Na2SO4The volume ratio of/NaOH mixed solutions is 2.8 ~ 3.3:1, the Na2SO4Na in/NaOH mixed solutions2SO4A concentration of 0.85 ~ 1.15mol/L, the Na2SO4NaOH concentration in/NaOH mixed solutions is 0.40 ~ 0.60mol/L;S2. the mixed system of S1. is aged, aging condition is 87 ~ 93 DEG C, 75 ~ 85h of time, collects precipitation, as alkali magnesium sulfate crystal whisker.The preparation method of the present invention removes complicated dedoping step from, can efficiently, high level, environmentally protective develop and use salt lake and saltern magnesium resource;And alkali magnesium sulfate crystal whisker yield is high, and it is best in quality, it prepares magnesium salt whisker on a large scale suitable for actual production, there is huge application value.
Description
Technical field
The present invention relates to alkali magnesium sulfate crystal whisker technical fields, and Hoh Yanhu making from brine is utilized more particularly, to a kind of
The method of standby alkali magnesium sulfate crystal whisker.
Background technology
Using Hoh Yanhu making from brine for the prior art of alkali magnesium sulfate crystal whisker, generally require by complicated except general labourer
Attention is generally placed on and how first to remove brine impurity by skill, technical staff, then goes to prepare expected material or side again
Prepare side removal of impurities or first tentatively obtained crude product, then go removal of impurities etc..It is either any, due to there is complicated removal of impurities,
Damage will be brought to environment.So this " not utilizing using destruction Of resources environment or the good environment of protection of resources "
Contradictory relation becomes the technical bottleneck problem to develop and use Brine resources, is also difficult to utilize Ke efficient, environmentally protectively now
Ke's salt lake bittern prepares alkali magnesium sulfate crystal whisker.
Invention content
The present invention is the defects of overcoming described in the above-mentioned prior art, provides a kind of utilization Hoh Yanhu making from brine for alkali formula sulphur
The method of sour magnesium whisker.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
It is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, include the following steps:
S1. it is 77 ~ 83 DEG C brine to be filtered and keep temperature, and Na is then added dropwise into brine under stiring2SO4/ NaOH is mixed
Solution obtains mixed system after dripping;The a concentration of of magnesium ion is 2.3 ~ 3.2 mol/L in the brine, the brine with
The Na2SO4The volume ratio of/NaOH mixed solutions is 2.8 ~ 3.3:1, the Na2SO4Na in/NaOH mixed solutions2SO4It is dense
It spends for 0.85 ~ 1.15mol/L, the Na2SO4NaOH concentration in/NaOH mixed solutions is 0.40 ~ 0.60mol/L;
S2. the mixed system of S1. is aged, aging condition is 87 ~ 93 DEG C, 75 ~ 85h of time, collects precipitation, as alkali
Formula magnesium sulfate crystal whisker.
When using Hoh Yanhu making from brine for alkali magnesium sulfate crystal whisker, when physical and chemical condition is suitble to, using alkali
" self-cleaning " of formula magnesium sulfate crystal whisker quick, efficiently, prepare alkali magnesium sulfate crystal whisker to green non-pollution.Alkali magnesium sulfate crystal whisker
Unique property, i.e. atomic arrangement high-sequential, intact filling seldom lack filling, difficult adsorbing contaminant, the difficult spy being infected with by impurity
Property, it is general to represent this unique property of alkali magnesium sulfate crystal whisker with " self-cleaning ".Using this characteristic, from Hoh Yanhu brine
Middle to remove complicated impurity removal process when preparing alkali magnesium sulfate crystal whisker from, this develops and uses not only high level resource, but also protecting ecology
Environment has important meaning.
The scientific basis of whisker self-cleaning is:First, as described above, whisker is defective without (or seldom containing);Second,
The whisker surface field of force is distributed in high degree of symmetry and specific surface area is small, thus is not easy adsorbing contaminant, according to surface chemistry theory, surface
The field of force is more symmetrical, specific surface area is smaller, to the adsorption capacity of impurity with regard to smaller, it is difficult to which chemisorbed occurs;Third, it is brilliant
It must require growth unit that must have specific stabilization energy in growth course, otherwise cannot enter lattice.But, the object of whisker
Reason absorption is on the contrary certainly existing, but this weak physical absorption need to only be washed with water and can remove the impurity of absorption.Herein
Spy explains, the whisker said herein for having self-cleaning, refers to thering is linear normal whisker, if whisker does not have straight line
Structure may not have self-cleaning.It, will be including normal whisker more intuitively to express this exclusive self-cleaning of whisker
Four kinds of common structures of matter are plotted in Fig. 1, and Fig. 1 intuitively expresses four kinds of structures of matter and impurity relationship.It can from Fig. 1-(a)
See, normal condition whisker surface is smooth, and column structure, macroscopic symmetry is very high, zero defect, therefore without adsorbing contaminant;Fig. 1-
(b) fusiform is represented, the substance of fusellal fabric also easily wraps up impurity;Fig. 1-(c) represents that general crystal can generate defect and introduce
Impurity, though being drawn as four directions in figure, what is represented is general crystal;Fig. 1-(d) represents colloid due to having big specific surface and pole
The asymmetric surface field of force and adsorb a large amount of impurity.Fig. 2 shows the self-cleaning (left side) without utilizing whisker with utilizing whisker
Self-cleaning (right side) comparison.As can be seen from Figure 2, not using the self-cleaning of whisker, then more " complicated removal of impurities " techniques, no
But production cost is improved, and has injured environment;If using the self-cleaning of whisker, complicated dedoping step is eliminated, is made
Production line simplifies, cost reduction, and to environment without any injury.But must explicitly point out herein, alkali magnesium sulfate is brilliant
Must have ready conditions requirement with self-cleaning, be not that can all be produced from clean property at any time.The brine in salt lake is complicated
Dense salt system, the type of inorganic salts and its content are generally different in the brine in different salt lakes, prepare alkali magnesium sulfate needs
The condition of self-cleaning is also entirely different, needs to pay the condition that huge research effort is possible to obtain self-cleaning.
Preferably, the Na in step S1.2SO4The rate of addition of/NaOH mixed solutions is to be dripped off in 1 ~ 2min
80mL.It needs to control rate of addition, prevents local base concentration excessively high, lead to flocculent deposit;Speed is generally in 1 ~ 2min and drips off
80mL, that is, 40 ~ 80mL/min;General rate of addition and Na2SO4NaOH concentration is in inverse ratio, NaOH in/NaOH mixed solutions
Concentration is high, then rate of addition needs slow down.
Preferably, the Na2SO4/ NaOH mixed solutions use the first Na of 1.70 ~ 2.30mol/L2SO4Solution and 0.80
The NaOH solution of ~ 1.20mol/L mixes in equal volume.
Preferably, brine described in step S1. is kept the temperature using heating water bath.Using heating water bath, it is heated evenly.
Preferably, mixed system described in step S2. is kept the temperature using heating water bath.
Preferably, the method further includes drying operation, it is described be deposited in 77 ~ 83 DEG C under the conditions of dry 23 ~ 25h.It can be with
It is dried using baking oven, drying temperature is set as 80 DEG C ± 3 DEG C, and general drying is for 24 hours.
It is highly preferred that the method further includes the 2nd Na2SO4Solution treatment processing step, the precipitation is through the 2nd Na2SO4
It is dried again after solution treatment.There may be a small amount of basic magnesium chloride whisker to be coexisted with alkali magnesium sulfate crystal whisker in product, it can
Use Na2SO4Solution treatment can obtain the higher alkali magnesium sulfate crystal whisker of purity.
Preferably, the 2nd Na2SO4A concentration of 2.000mol/L ± 0.3mol/L of solution.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention utilizes the self-cleaning of alkali magnesium sulfate crystal whisker, by controlling Na2SO4The concentration of/NaOH mixed solutions and addition
Volume and bath temperature, Aging Temperature, digestion time can be produced to obtain using Hoh Yanhu brine with meeting the requirements
Whisker purity alkali magnesium sulfate crystal whisker.Remove complicated dedoping step from, can efficiently, high level, environmentally protective develop and use
Salt lake and saltern magnesium resource;And alkali magnesium sulfate crystal whisker yield is high, and it is best in quality, it is prepared on a large scale suitable for actual production
Magnesium salt whisker has huge application value.
Description of the drawings
Fig. 1 is four kinds of structures of matter and the relationship of impurity, and figure orbicular spot represents impurity.
In Fig. 1, the whisker of (a) normal condition, (b) fusiform whisker, (c) general crystal, (d) amorphous substance.
Fig. 2 is without the self-cleaning using whisker(It is left)With the self-cleaning using whisker(It is right)Comparison schematic diagram.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
In the result of embodiment 1 ~ 4 and comparative example 1 ~ 12, whisker ratio is using flying-spot microscope observation estimation, result
Mass fraction;Whisker draw ratio also is observed to obtain using flying-spot microscope;
It should be noted that alkali magnesium sulfate crystal whisker generally requires draw ratio to be not less than 10:1;But, the requirement draw ratio also having
Not less than 5:1.
Embodiment 1
It is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, include the following steps
S1. 300mL Hoh Yanhu brine is taken, filter and discards insoluble matter, magnesium ion concentration is 3.0 mol/L;
S2. the first Na of 2.000mol/L is prepared2SO4The NaOH solution of solution and 1.000mol/L, then isometric mixing,
Referred to as Na2SO4/ NaOH mixed solutions;
S3. Hoh Yanhu brine 150mL is taken to be placed in the conical flask of 250mL, and conical flask is built in 80 DEG C of water-bath heating
It to 80 DEG C and keeps the temperature, is then slowly added dropwise under stirring into Na2SO4/ NaOH mixed solutions 53.5mL(That is, bittern with
Na2SO4The volume ratio of/NaOH mixed solutions is 2.8:1), rate of addition 40mL/min obtains mixed system;
S4. the mixed system of S3. is placed in water temperature is after continuing to be aged 80h in 90 DEG C of water-bath, and when ageing can be given suitable
When stirring, precipitation is collected by filtration, is placed in baking oven(80 DEG C, for 24 hours)Drying is to get alkali magnesium sulfate crystal whisker;It may in product
There is a small amount of basic magnesium chloride whisker to be coexisted with alkali magnesium sulfate crystal whisker, the second Na can be used2SO4Solution treatment can obtain purity compared with
High alkali magnesium sulfate crystal whisker, the 2nd Na2SO4A concentration of 2.000 mol/L of solution.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 22:1, whisker ratio is 97%.
Embodiment 2
The present embodiment using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, include the following steps
S1. 300mL Hoh Yanhu brine is taken, filter and discards insoluble matter, magnesium ion concentration is 2.3 mol/L;
S2. the first Na of 1.700mol/L is prepared2SO4The NaOH solution of solution and 1.200mol/L, then isometric mixing,
Referred to as Na2SO4/ NaOH mixed solutions;
S3. Hoh Yanhu brine 150mL is taken to be placed in the conical flask of 250mL, and conical flask is built in 83 DEG C of water-bath heating
It to 83 DEG C and keeps the temperature, is then slowly added dropwise under stirring into Na2SO4/ NaOH mixed solutions 53.5mL(That is, bittern with
Na2SO4The volume ratio of/NaOH mixed solutions is 2.8:1), rate of addition 60mL/min obtains mixed system;
S4. the mixed system of S3. is placed in water temperature is after continuing to be aged 85h in 87 DEG C of water-bath, and when ageing can be given suitable
When stirring, precipitation is collected by filtration, is placed in baking oven(77 DEG C, 25h)Drying is to get alkali magnesium sulfate crystal whisker;It may in product
There is a small amount of basic magnesium chloride whisker to be coexisted with alkali magnesium sulfate crystal whisker, the second Na can be used2SO4Solution treatment can obtain purity compared with
High alkali magnesium sulfate crystal whisker, the 2nd Na2SO4A concentration of 2.300mol/L of solution.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 21:1, whisker ratio is 98%.
Embodiment 3
The present embodiment using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, include the following steps
S1. 300mL Hoh Yanhu brine is taken, filter and discards insoluble matter, magnesium ion concentration is 2.6 mol/L;
S2. the first Na of 2.000mol/L is prepared2SO4The NaOH solution of solution and 0.800mol/L, then isometric mixing,
Referred to as Na2SO4/ NaOH mixed solutions;
S3. Hoh Yanhu brine 150mL is taken to be placed in the conical flask of 250mL, and conical flask is built in 77 DEG C of water-bath heating
It to 77 DEG C and keeps the temperature, is then slowly added dropwise under stirring into Na2SO4/ NaOH mixed solutions 50.0mL(That is, bittern with
Na2SO4The volume ratio of/NaOH mixed solutions is 3.0:1), until rate of addition is 80mL/min, obtain mixed system;
S4. the mixed system of S3. is placed in water temperature is after continuing to be aged 75h in 87 DEG C of water-bath, and when ageing can be given suitable
When stirring, precipitation is collected by filtration, is placed in baking oven(80 DEG C, 25h)Drying is to get alkali magnesium sulfate crystal whisker;It may in product
There is a small amount of basic magnesium chloride whisker to be coexisted with alkali magnesium sulfate crystal whisker, the second Na can be used2SO4Solution treatment can obtain purity compared with
High alkali magnesium sulfate crystal whisker, the 2nd Na2SO4A concentration of 1.700 mol/L of solution.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 20:1, whisker ratio is 96%.
Embodiment 4
The present embodiment using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, include the following steps
S1. 300mL Hoh Yanhu brine is taken, filter and discards insoluble matter, magnesium ion concentration is 3.2 mol/L;
S2. the first Na of 2.300mol/L is prepared2SO4The NaOH solution of solution and 0.800mol/L, then isometric mixing,
Referred to as Na2SO4/ NaOH mixed solutions;
S3. Hoh Yanhu brine 150mL is taken to be placed in the conical flask of 250mL, and conical flask is built in 80 DEG C of water-bath heating
It to 80 DEG C and keeps the temperature, is then slowly added dropwise under stirring into Na2SO4/ NaOH mixed solutions 45.5mL(That is, bittern with
Na2SO4The volume ratio of/NaOH mixed solutions is 3.3:1), rate of addition 60mL/min obtains mixed system;
S4. the mixed system of S3. is placed in water temperature is after continuing to be aged 75h in 93 DEG C of water-bath, and when ageing can be given suitable
When stirring, precipitation is collected by filtration, is placed in baking oven(83 DEG C, 23h)Drying is to get alkali magnesium sulfate crystal whisker;It may in product
There is a small amount of basic magnesium chloride whisker to be coexisted with alkali magnesium sulfate crystal whisker, the second Na can be used2SO4Solution treatment can obtain purity compared with
High alkali magnesium sulfate crystal whisker, the 2nd Na2SO4A concentration of 1.700 mol/L of solution.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 22:1, whisker ratio is 97%.
Comparative example 1
Difference lies in bittern and Na in S3. with embodiment 12SO4The volume ratio of/NaOH mixed solutions is 4.5:1.
Other raw materials and operating procedure are same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 13:1, whisker ratio is 20%.
Comparative example 2
Difference lies in bittern and Na in S3. with embodiment 12SO4The volume ratio of/NaOH mixed solutions is 1.9:1;
Other raw materials and operating procedure are same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 12:1, whisker ratio is 20%.
Comparative example 3
Difference lies in Na with embodiment 12SO4The Na of/NaOH mixed solutions2SO4A concentration of 1.900mol/L, other raw materials and
Operating procedure is same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 16:1, whisker ratio is 12%.
Comparative example 4
Difference lies in Na with embodiment 12SO4The Na of/NaOH mixed solutions2SO4A concentration of 0.300mol/L, other raw materials and
Operating procedure is same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 4:1, whisker ratio is 1.3%.
Comparative example 5
Difference lies in Na with embodiment 12SO4The NaOH concentration of/NaOH mixed solutions be 1.200mol/L, other raw materials and
Operating procedure is same as Example 1.
As a result:No whisker generation.
Comparative example 6
Difference lies in Na with embodiment 12SO4The NaOH concentration of/NaOH mixed solutions be 0.200mol/L, other raw materials and
Operating procedure is same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 8:1, whisker ratio is 1.2%.
Comparative example 7
Difference lies in the bath temperature of brine is 96 DEG C in S3., other raw materials and operating procedure and embodiment 1 with embodiment 1
It is identical.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 8:1, whisker ratio is 26%.
Comparative example 8
Difference lies in the bath temperature of brine is 55 DEG C in S3., other raw materials and operating procedure and embodiment 1 with embodiment 1
It is identical.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 13:1, whisker ratio is 31%.
Comparative example 9
Difference lies in the bath temperatures of mixed system in S4. with embodiment 1(That is Aging Temperature)It is 96 DEG C;Other raw materials and
Operating procedure is same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 16:1, whisker ratio is 18%.
Comparative example 10
Difference lies in the bath temperatures of mixed system in S4. with embodiment 1(That is Aging Temperature)It is 60 DEG C;Other raw materials and
Operating procedure is same as Example 1.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 9:1, whisker ratio is 12%.
Comparative example 11
Difference lies in the digestion time of mixed system is 20h, other raw materials and operating procedure and implementation in S4. with embodiment 1
Example 1 is identical.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 6:1, whisker ratio is 8%.
Comparative example 12
Difference lies in the digestion time of mixed system is 30h, other raw materials and operating procedure and implementation in S4. with embodiment 1
Example 1 is identical.
Alkali magnesium sulfate crystal whisker draw ratio obtained is 8:1, whisker ratio is 16%.
According to the experimental result of embodiment 1 ~ 4 and comparative example 1 ~ 12 it is found that energy under conditions of the embodiment of the present invention 1 ~ 4
Whisker " self-cleaning " is enough generated, whisker ratio is high in product obtained, and draw ratio is very excellent, can be prepared excellent
Alkali magnesium sulfate crystal whisker.And product whisker ratio prepared by comparative example 1 ~ 12 is very low, the substance of non-whisker is more, and some is even
Whisker cannot be generated.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
All any modification, equivalent and improvement made within the spirit and principle of invention etc., should be included in the claims in the present invention
Protection domain within.
Claims (7)
1. it is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker, which is characterized in that include the following steps:
S1. it is 77 ~ 83 DEG C brine to be filtered and keep temperature, and Na is then added dropwise into brine under stiring2SO4/ NaOH mixing is molten
Liquid obtains mixed system after dripping;A concentration of 2.3 ~ 3.2mol/L of magnesium ion in the brine, the brine with it is described
Na2SO4The volume ratio of/NaOH mixed solutions is 2.8 ~ 3.3:1, the Na2SO4Na in/NaOH mixed solutions2SO4It is a concentration of
0.85 ~ 1.15mol/L, the Na2SO4NaOH concentration in/NaOH mixed solutions is 0.40 ~ 0.60mol/L;
S2. the mixed system of S1. is aged, aging condition is 87 ~ 93 DEG C, 75 ~ 85h of time, collects precipitation, as alkali
Formula magnesium sulfate crystal whisker.
2. the according to the method described in claim 1, it is characterized in that, Na in step S1.2SO4/ NaOH mixed solutions
Rate of addition is that 80mL is dripped off in 1 ~ 2min.
3. the according to the method described in claim 1, it is characterized in that, Na2SO4/ NaOH mixed solutions using 1.70 ~
The first Na of 2.30mol/L2SO4The NaOH solution of solution and 0.80 ~ 1.20mol/L mix in equal volume.
4. according to the method described in claim 1, it is characterized in that, brine described in step S1. is kept the temperature using heating water bath.
5. according to the method described in claim 1, it is characterized in that, mixed system described in step S2. is protected using heating water bath
Temperature.
It is 6. described to be deposited in 77 ~ 83 DEG C of conditions according to the method described in claim 1, it is characterized in that, further include drying operation
23 ~ 25h of lower drying.
7. according to the method described in claim 6, it is characterized in that, further include the 2nd Na2SO4Solution treatment processing step, it is described
Precipitation is through the 2nd Na2SO4It is dried again after solution treatment.
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Citations (3)
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CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
CN103789819A (en) * | 2014-02-19 | 2014-05-14 | 中国科学院青海盐湖研究所 | Preparation method of fibrous alkali magnesium sulfate whisker |
CN103806090A (en) * | 2012-11-15 | 2014-05-21 | 毛其伟 | Preparation method of basic magnesium sulfate whisker |
-
2017
- 2017-12-25 CN CN201711423193.1A patent/CN108166062A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
CN103806090A (en) * | 2012-11-15 | 2014-05-21 | 毛其伟 | Preparation method of basic magnesium sulfate whisker |
CN103789819A (en) * | 2014-02-19 | 2014-05-14 | 中国科学院青海盐湖研究所 | Preparation method of fibrous alkali magnesium sulfate whisker |
Non-Patent Citations (1)
Title |
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吴健松等: "徐闻盐场苦卤制备碱式硫酸镁晶须", 《无机盐工业》 * |
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