CN109133134A - A kind of preparation method of high-purity strontium hydroxide - Google Patents
A kind of preparation method of high-purity strontium hydroxide Download PDFInfo
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- CN109133134A CN109133134A CN201811306192.3A CN201811306192A CN109133134A CN 109133134 A CN109133134 A CN 109133134A CN 201811306192 A CN201811306192 A CN 201811306192A CN 109133134 A CN109133134 A CN 109133134A
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- strontium hydroxide
- strontium
- hydroxide
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- hot solution
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- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 title claims abstract description 128
- 229910001866 strontium hydroxide Inorganic materials 0.000 title claims abstract description 127
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000047 product Substances 0.000 claims abstract description 42
- 239000012043 crude product Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- SYJBLFMEUQWNFD-UHFFFAOYSA-N magnesium strontium Chemical compound [Mg].[Sr] SYJBLFMEUQWNFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000001681 protective effect Effects 0.000 claims abstract description 13
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 229910052712 strontium Inorganic materials 0.000 claims description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 10
- -1 cerium hydroxide strontium Chemical compound 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims 3
- 239000001301 oxygen Substances 0.000 claims 3
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 abstract description 19
- 229910000018 strontium carbonate Inorganic materials 0.000 abstract description 19
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000003763 carbonization Methods 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 description 21
- 239000013078 crystal Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 10
- 238000009835 boiling Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 6
- 230000003292 diminished effect Effects 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- CZMRCDWAGMRECN-UHFFFAOYSA-N Rohrzucker Natural products OCC1OC(CO)(OC2OC(CO)C(O)C(O)C2O)C(O)C1O CZMRCDWAGMRECN-UHFFFAOYSA-N 0.000 description 1
- 229920001617 Vinyon Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical class [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- 150000003438 strontium compounds Chemical class 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Inorganic materials [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 description 1
- WJMMDJOFTZAHHS-UHFFFAOYSA-L strontium;carbonic acid;carbonate Chemical compound [Sr+2].OC([O-])=O.OC([O-])=O WJMMDJOFTZAHHS-UHFFFAOYSA-L 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
- C01F11/16—Purification
-
- 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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
- C01F11/04—Oxides or hydroxides by thermal decomposition
- C01F11/06—Oxides or hydroxides by thermal decomposition of carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of high-purity strontium hydroxide, comprising: S1, calcines industrial magnesium strontium by microwave calcination method, obtains calcined product；S2, water logging calcined product simultaneously carry out heat filtering, obtain the first strontium hydroxide hot solution；S3, cooling first strontium hydroxide hot solution to crystallization, and be separated by solid-liquid separation, dry gained solid phase obtains strontium hydroxide crude product；S4, under protective atmosphere, strontium hydroxide crude product is recrystallized, high-purity strontium hydroxide is obtained；Wherein, the content of Strontia hydrate is not less than 99.5% in high-purity strontium hydroxide.The present invention passes through to be recrystallized under microwave calcination method join protection atmosphere; on the one hand the quick burning to industrial magnesium strontium is realized; calcination efficiency greatly improved; on the other hand also maximumlly reduce the carbonization for the strontium hydroxide being subsequently generated; reduce the content of strontium carbonate impurity in final strontium hydroxide product; make Strontium carbonate contents lower than 0.3%, effectively increases the purity of strontium hydroxide product.
Description
Technical field
The invention belongs to strontium hydroxide preparation technical fields, it relates in particular to a kind of preparation side of high-purity strontium hydroxide
Method.
Background technique
Strontium hydroxide is a kind of important strontium compound product, is widely used in the refining processing of beet sugar earliest,
Furthermore it also serves as the stabilizer of vinyon, is used for strontium lubricating wax, and the drying property for improving drying oil and paint
Deng；Strontium hydroxide is also the intermediate compound or raw material for preparing other strontium products.
The preparation method of strontium hydroxide includes by raw material of celestine and using strontium carbonate as raw material two major classes, wherein with carbonic acid
Strontium carbonate acidization can be used when being raw material in strontium.
Strontium carbonate acidization be obtain strontium chloride solution or strontium nitrate solution with hydrochloric acid or nitric acid dissolution industrial magnesium strontium, then
The impurity such as iron therein are removed, sodium hydroxide reactive crystallization is eventually adding and obtains Strontia hydrate product.Strontium carbonate acidization
Process flow is as follows: being first beaten useless strontium carbonate, is slowly added to nitric acid, stirs to fully reacting, then use hydroxide
Sodium adjusts pH, makes pH >=7.5 of mixed liquor；Then mixed liquor is heated to 80 DEG C~90 DEG C, is filtered, washed after keeping the temperature 30min,
Obtain strontium nitrate solution；Finally sodium hydroxide is dissolved, strontium nitrate solution is slowly added under stirring, after fully reacting, is cooled to
Thick Strontia hydrate is obtained by filtration in room temperature, by Strontia hydrate by recrystallizing, being dried to obtain Strontia hydrate.
But more or less all contain some strontium carbonates in the strontium hydroxide product prepared in the prior art, while right
The impurity content of strontium carbonate in strontium hydroxide product, relevant industries standard, company standard are not all done clearly stipulate that even having
Think that strontium carbonate is qualification not higher than 2% in a little analysis pure cerium hydroxide strontium reagents, therefore universal in strontium hydroxide product at present
Containing strontium carbonate, Strontium carbonate contents are between 1%~2%.
Summary of the invention
To solve the problems, such as that above-mentioned strontium hydroxide product purity of the existing technology is not high, the present invention provides a kind of high
The preparation method of pure cerium hydroxide strontium.
In order to achieve the above object of the invention, present invention employs the following technical solutions:
A kind of preparation method of high-purity strontium hydroxide, comprising the following steps:
S1, industrial magnesium strontium is calcined by microwave calcination method, obtains calcined product.
Calcined product described in S2, water logging simultaneously carries out heat filtering, obtains the first strontium hydroxide hot solution.
S3, the cooling first strontium hydroxide hot solution to crystallization, and be separated by solid-liquid separation, dry gained solid phase obtains
Strontium hydroxide crude product；Wherein, the content of Strontia hydrate is not less than 99% in the strontium hydroxide crude product.
S4, under protective atmosphere, the strontium hydroxide crude product is recrystallized, high-purity strontium hydroxide is obtained；Wherein, institute
The content of Strontia hydrate in high-purity strontium hydroxide is stated not less than 99.5%.
Further, in the step S1, calcination temperature be 1250 DEG C~1350 DEG C, calcination time be 10min~
30min。
Further, the specific method of the step S4 includes:
S41, under protective atmosphere, dissolve the strontium hydroxide crude product and carry out heat filtering, obtain the second strontium hydroxide heat
Solution.
S42, under protective atmosphere, the cooling second strontium hydroxide hot solution is separated by solid-liquid separation to crystallizing, dry
Gained solid phase obtains high-purity strontium hydroxide.
Further, the protective atmosphere is N2, Ar, He atmosphere.
Further, in the step S41, dissolve after the strontium hydroxide crude product and the 10min~30min that boils again into
Row heat filtering, to obtain the second strontium hydroxide hot solution.
Further, in the step S41, the strontium hydroxide crude product is dissolved according to the solid-to-liquid ratio of 1:4~1:8.
Further, in the step S42, the cooling second strontium hydroxide hot solution is to 5 DEG C~25 DEG C, to carry out
Crystallization.
Further, in the step S2, heat is carried out again after calcined product described in water logging and the 10min~30min that boils
Filtering, to obtain the first strontium hydroxide hot solution.
Further, in the step S2, calcined product described in the solid-to-liquid ratio water logging according to 1:5~1:10.
Further, in the step S3, the cooling first strontium hydroxide hot solution is to 5 DEG C~25 DEG C, to carry out
Crystallization.
The present invention, which passes through, carries out recrystallization purification under microwave calcination method join protection atmosphere, on the one hand realizes to industrial carbon
The quick burning of sour strontium greatly improved calcination efficiency, on the other hand also maximumlly reduce the strontium hydroxide being subsequently generated
Carbonization, reduce the content of strontium carbonate impurity in final strontium hydroxide product, effectively increase the purity of strontium hydroxide product；Root
The content of Strontia hydrate can reach 99.5% or more, and carbon in the high-purity strontium hydroxide obtained according to preparation method of the invention
Sour strontium impurity content is controllable to be lower than 0.3%, be it is a kind of using the industrial magnesium strontium of low cost as raw material it is completely new prepare it is high-purity
The new method of strontium hydroxide, and its simple process also avoid not can cause environmental pollution using hydrochloric acid and sodium hydroxide etc..
Detailed description of the invention
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing:
Fig. 1 is the XRD result of the one high-purity strontium hydroxide of gained of embodiment.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to come in many different forms real
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, providing these implementations
Example is in order to explain the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
Term " first ", " second " etc. herein can be used to describe various substances although will be appreciated that, these
Substance should not be limited by these terms.These terms are only used to distinguish a substance with another substance.
The present inventor is based on purity and the preparation side that not can guarantee high-purity strontium hydroxide generally in the prior art
The technical problems such as many drawbacks in method provide using industrial magnesium strontium as raw material and a kind of completely new prepare high-purity strontium hydroxide
Method.
The preparation method of high-purity strontium hydroxide of the invention the following steps are included:
In step sl, industrial magnesium strontium is calcined by microwave calcination method, obtains calcined product.
Preferably, in this step, calcination temperature is 1250 DEG C~1350 DEG C, and calcination time is 10min~30min.It is micro-
Wave heating can achieve the effect of quick burning, and the required time is Muffle furnace, electric furnace, tunnel oven, elevator kiln, rotary kiln
Etc. equipment heating time the part of part even ten.
In step s 2, water logging calcined product and heat filtering is carried out, obtains the first strontium hydroxide hot solution.
Preferably, in this step, according to the solid-to-liquid ratio water logging calcined product of 1:5~1:10；That is, every 1 mass
The calcined product of part then utilizes the water of 5~10 mass parts to carry out water logging.
It is further preferred that in this step, heat filtering is carried out again after water logging calcined product and the 10min~30min that boils,
To obtain the first strontium hydroxide hot solution.
In step s3, cooling first strontium hydroxide hot solution extremely crystallizes, and is separated by solid-liquid separation, dry gained solid phase,
Obtain strontium hydroxide crude product.
Specifically, the content of Strontia hydrate is not less than 99% in obtained strontium hydroxide crude product.
Preferably, in this step, cooling first strontium hydroxide hot solution is to 5 DEG C~25 DEG C, to be crystallized.
In this way, realizing i.e. by first time water logging-heat filtering-crystallisation by cooling-filtering and separating strontium money from calcined product
The purpose in source is separated strontium resource in the form of strontium hydroxide crude product with the other impurities in calcined product.
In step s 4, under protective atmosphere, strontium hydroxide crude product is recrystallized, obtains high-purity strontium hydroxide.
Specifically, the content of Strontia hydrate is not less than 99.5% in obtained high-purity strontium hydroxide.
Preferably, the protective atmosphere is N2, Ar, He atmosphere.It can maximumlly be reduced by the way of atmosphere protection
The carbonization of strontium hydroxide guarantees the high-purity of subsequent product.
More specifically, the method for the step includes operations described below: (1) under protective atmosphere, dissolving strontium hydroxide crude product
And heat filtering is carried out, obtain the second strontium hydroxide hot solution；(2) under protective atmosphere, cooling the second strontium hydroxide heat obtained
Solution extremely crystallizes, and is separated by solid-liquid separation, dry gained solid phase obtains above-mentioned high-purity strontium hydroxide.
Further, strontium hydroxide crude product is dissolved according to the solid-to-liquid ratio of 1:4~1:8.
And heat filtering is carried out again after preferably, dissolving strontium hydroxide crude product and the 10min~30min that boils, to obtain
State the second strontium hydroxide hot solution.
Further, in aforesaid operations, cooling second strontium hydroxide hot solution is to 5 DEG C~25 DEG C, to be crystallized.
Illustrate the preparation method of above-mentioned high-purity strontium hydroxide of the invention, but ability below with reference to specific embodiment
Field technique personnel will be understood by, and following embodiments are only the specific examples of above-mentioned preparation method, be not limited to its whole.
Embodiment one
The first step calcines strontium carbonate.
Specifically, 200g industrial magnesium strontium is weighed, is placed it in microwave calcination furnace, 15min is warming up to 1250 DEG C, protects
Warm 30min obtains calcined product 140.5g.
Second step prepares strontium hydroxide crude product.
Specifically, calcined product and 702.5g water are subjected to water logging, are heated to the 10min that boils and keep, obtain first
Slurry；The first slurry is filtered while hot and obtains the first strontium hydroxide hot solution, which is cooled to 5 DEG C, separation of solid and liquid obtains
Obtain aqueous Strontia hydrate crude crystalline；The crystal is placed in air dry oven, dry 30min under the conditions of 50 DEG C,
Obtain strontium hydroxide crude product 325g.
In the strontium hydroxide crude product of acquisition, the content of Strontia hydrate is 98.93%.
Third step prepares high-purity strontium hydroxide.
Specifically, 200g strontium hydroxide crude product and 800g water are weighed in N2It is dissolved under atmosphere, is heated to boiling simultaneously
10min is kept, the second slurry is obtained；It is filtered under diminished pressure the second slurry and obtains the second strontium hydroxide hot solution, by the solution in N2Gas
It is cooled under atmosphere to 5 DEG C, is quickly separated by solid-liquid separation and obtains aqueous strontium hydroxide crystal；The crystal is placed in vacuum drying
In case, dry 30min, obtains 185.2g product under the conditions of 30 DEG C.
The product obtained to the embodiment has carried out X-ray diffraction test (XRD), and XRD result is as shown in Figure 1.By Fig. 1
It is compareed with Strontia hydrate standard card (PDF98-041-7100), learns the diffraction maximum and the standard card in Fig. 1
Diffraction maximum it is consistent, no miscellaneous peak occurs, it can thus be appreciated that the product that the present embodiment obtains is mainly Strontia hydrate.And through dividing
Analysis, wherein the content of Strontia hydrate is 99.57%, and wherein Strontium carbonate contents are 0.28%, belongs to a kind of high-purity hydroxide
Strontium.
Embodiment two
The first step calcines strontium carbonate.
Specifically, 200g industrial magnesium strontium is weighed, is placed in microwave calcination furnace, 15min is warming up to 1280 DEG C, heat preservation
25min obtains calcined product 141.5g.
Second step prepares strontium hydroxide crude product.
Specifically, calcined product and 849g water are subjected to water logging, are heated to the 15min that boils and keep, obtain the first slurry
Material；The first slurry is filtered while hot and obtains the first strontium hydroxide hot solution, which is cooled to 10 DEG C；It is separated by solid-liquid separation and obtains
Aqueous Strontia hydrate crude crystalline；The crystal is placed in air dry oven, dry 30min, is obtained under the conditions of 50 DEG C
Obtain strontium hydroxide crude product 306g.
In the strontium hydroxide crude product of acquisition, the content of Strontia hydrate is 99.01%.
Third step prepares high-purity strontium hydroxide.
Specifically, it weighs strontium hydroxide crude product 200g and 1000g water to be dissolved under an ar atmosphere, is heated to boiling simultaneously
15min is kept, the second slurry is obtained；It is filtered under diminished pressure the second slurry and obtains the second strontium hydroxide hot solution, by the solution in Ar gas
It is cooled under atmosphere to 10 DEG C, is quickly separated by solid-liquid separation and obtains aqueous strontium hydroxide crystal；The crystal is placed in vacuum to do
In dry case, dry 30min, obtains high-purity strontium hydroxide 169.7g, wherein the content of Strontia hydrate is under the conditions of 25 DEG C
99.63%, wherein Strontium carbonate contents are 0.23%.
Embodiment three
The first step calcines strontium carbonate.
Specifically, 200g industrial magnesium strontium is weighed, is placed in microwave calcination furnace, 15min is warming up to 1300 DEG C, heat preservation
20min obtains calcined product 140.3g.
Second step prepares strontium hydroxide crude product.
Specifically, calcined product and 982g water are subjected to water logging, are heated to the 20min that boils and keep, obtain the first slurry
Material；The first slurry is filtered while hot and obtains the first strontium hydroxide hot solution, which is cooled to 15 DEG C, is separated by solid-liquid separation and is obtained
Aqueous Strontia hydrate crude crystalline；The crystal is placed in air dry oven, dry 30min, is obtained under the conditions of 50 DEG C
Obtain strontium hydroxide crude product 300.5g.
In the strontium hydroxide crude product of acquisition, the content of Strontia hydrate is 99.03%.
Third step prepares high-purity strontium hydroxide.
Specifically, it weighs strontium hydroxide crude product 200g and 1200g water to be dissolved under He atmosphere, is heated to boiling simultaneously
20min is kept, the second slurry is obtained；It is filtered under diminished pressure the second slurry and obtains the second strontium hydroxide hot solution, by the solution in He gas
It is cooled under atmosphere to 15 DEG C, is quickly separated by solid-liquid separation and obtains aqueous strontium hydroxide crystal；The crystal is placed in vacuum to do
In dry case, dry 30min, obtains high-purity strontium hydroxide 166.1g, wherein the content of Strontia hydrate is under the conditions of 30 DEG C
99.79%, wherein Strontium carbonate contents 0.19%.
Example IV
The first step prepares strontium oxide strontia.
Specifically, 200g industrial magnesium strontium is weighed, is placed in microwave calcination furnace, 15min is warming up to 1320 DEG C, heat preservation
15min obtains calcined product 140.8g.
Second step prepares strontium hydroxide crude product.
Specifically, calcined product and 1267g water are subjected to water logging, are heated to the 25min that boils and keep, obtain the first slurry
Material；The first slurry is filtered while hot and obtains the first strontium hydroxide hot solution, which is cooled to 20 DEG C, is separated by solid-liquid separation and is obtained
Aqueous Strontia hydrate crude crystalline；The crystal is placed in air dry oven, dry 30min, is obtained under the conditions of 50 DEG C
Obtain strontium hydroxide crude product 286g.
In the strontium hydroxide crude product of acquisition, the content of Strontia hydrate is 98.98%.
Third step prepares high-purity strontium hydroxide.
Specifically, strontium hydroxide crude product 200g and 1400g water are weighed in N2It is dissolved under atmosphere, is heated to boiling simultaneously
10min is kept, the second slurry is obtained；It is filtered under diminished pressure the second slurry and obtains the second strontium hydroxide hot solution, by the solution in N2Gas
It is cooled under atmosphere to 20 DEG C, is quickly separated by solid-liquid separation and obtains aqueous strontium hydroxide crystal；The crystal is placed in vacuum to do
In dry case, dry 30min, obtains high-purity strontium hydroxide 161.9g, wherein the content of Strontia hydrate is under the conditions of 30 DEG C
99.68%, wherein Strontium carbonate contents 0.18%.
Embodiment five
The first step prepares strontium oxide strontia.
Specifically, 200g industrial magnesium strontium is weighed, is placed in microwave calcination furnace, 15min is warming up to 1350 DEG C, heat preservation
10min obtains calcined product 141.2g.
Second step prepares strontium hydroxide crude product.
Specifically, calcined product and 1412g water are subjected to water logging, obtain strontium hydroxide slurry and are heated to boiling and protect
30min is held, the first slurry is obtained；Filter while hot the first slurry obtain heat strontium hydroxide solution, by the solution cool to
It 25 DEG C, is separated by solid-liquid separation and obtains aqueous Strontia hydrate crude crystalline；The crystal is placed in air dry oven, in 50 DEG C of items
Dry 30min, obtains strontium hydroxide crude product 277g under part.
In the strontium hydroxide crude product of acquisition, the content of Strontia hydrate is 98.92%.
Third step prepares high-purity strontium hydroxide.
Specifically, it weighs strontium hydroxide crude product 200g and 1600g water to be dissolved under an ar atmosphere, is heated to boiling simultaneously
30min is kept, the second slurry is obtained；It is filtered under diminished pressure the second slurry and obtains the second strontium hydroxide hot solution, by the solution in Ar gas
It is cooled under atmosphere to 25 DEG C, is quickly separated by solid-liquid separation and obtains aqueous strontium hydroxide crystal；The crystal is placed in vacuum to do
In dry case, dry 30min, obtains high-purity strontium hydroxide 151g, wherein the content of Strontia hydrate is under the conditions of 30 DEG C
99.81%, wherein Strontium carbonate contents 0.15%.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (10)
1. a kind of preparation method of high-purity strontium hydroxide, which comprises the following steps:
S1, industrial magnesium strontium is calcined by microwave calcination method, obtains calcined product；
Calcined product described in S2, water logging simultaneously carries out heat filtering, obtains the first strontium hydroxide hot solution；
S3, the cooling first strontium hydroxide hot solution to crystallization, and be separated by solid-liquid separation, dry gained solid phase obtains hydrogen-oxygen
Change strontium crude product；Wherein, the content of Strontia hydrate is not less than 99% in the strontium hydroxide crude product；
S4, under protective atmosphere, the strontium hydroxide crude product is recrystallized, high-purity strontium hydroxide is obtained；Wherein, the height
The content of Strontia hydrate is not less than 99.5% in pure cerium hydroxide strontium.
2. preparation method according to claim 1, which is characterized in that in the step S1, calcination temperature is 1250 DEG C
~1350 DEG C, calcination time is 10min~30min.
3. preparation method according to claim 1 or 2, which is characterized in that the specific method of the step S4 includes:
S41, under protective atmosphere, dissolve the strontium hydroxide crude product and carry out heat filtering, obtain the second strontium hydroxide hot solution；
S42, under protective atmosphere, the cooling second strontium hydroxide hot solution is separated by solid-liquid separation, dry gained to crystallizing
Solid phase obtains high-purity strontium hydroxide.
4. preparation method according to claim 3, which is characterized in that the protective atmosphere is N2, Ar, He atmosphere.
5. preparation method according to claim 3, which is characterized in that in the step S41, dissolve the strontium hydroxide
Heat filtering is carried out again after crude product and the 10min~30min that boils, to obtain the second strontium hydroxide hot solution.
6. preparation method according to claim 5, which is characterized in that in the step S41, according to consolidating for 1:4~1:8
Liquor ratio dissolves the strontium hydroxide crude product.
7. preparation method according to claim 3, which is characterized in that in the step S42, cooling second hydrogen-oxygen
Change strontium hot solution to 5 DEG C~25 DEG C, to be crystallized.
8. preparation method according to claim 3, which is characterized in that in the step S2, calcined product described in water logging
And heat filtering is carried out after the 10min~30min that boils again, to obtain the first strontium hydroxide hot solution.
9. preparation method according to claim 8, which is characterized in that in the step S2, according to consolidating for 1:5~1:10
Calcined product described in liquor ratio water logging.
10. preparation method according to claim 3, which is characterized in that in the step S3, cooling first hydrogen-oxygen
Change strontium hot solution to 5 DEG C~25 DEG C, to be crystallized.
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