CN108946782A - A method of preparing high-purity strontium fluoride in ethanol system - Google Patents
A method of preparing high-purity strontium fluoride in ethanol system Download PDFInfo
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- CN108946782A CN108946782A CN201811093150.6A CN201811093150A CN108946782A CN 108946782 A CN108946782 A CN 108946782A CN 201811093150 A CN201811093150 A CN 201811093150A CN 108946782 A CN108946782 A CN 108946782A
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- 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
- C01F11/20—Halides
- C01F11/22—Fluorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The present invention provides a kind of method that high-purity strontium fluoride is prepared in ethanol system, comprising the following steps: (1) prepared by strontium chloride solution: strontium chloride being dissolved in the mixed solution of ethyl alcohol and water, obtains strontium chloride solution；(2) crystallization reaction: strontium fluoride crystal seed is added in the strontium chloride solution obtained by step (1), while ammonium fluoride solution is added dropwise, is stirred for reacting after charging, obtains suspension；(3) it is filtered, washed: suspension obtained by step (2) is filtered, reusable heat water washing, filtering obtain strontium fluoride filter cake；(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is dried, and then at 400~500 DEG C, 3~4h of calcination crushes firing product, obtains high-purity strontium fluoride powder.The advantages that it can overcome drawbacks described above of the existing technology to the present invention, have impurity content low, and product purity is high, and production cost is low and high financial profit.
Description
Technical field
The present invention relates to a kind of methods for preparing high-purity strontium fluoride, and in particular to one kind prepares high-purity fluorine in ethanol system
Change the method for strontium.
Background technique
Strontium fluoride crystal is a kind of colorless and transparent cubic structure monocrystal, and optical property is very excellent, can be used for making
Make optical glass and laser monocrystalline.It can also be used in pharmaceuticals industry and daily chemical industry, solder flux, advanced electronic components etc..
Requirement of the preparation of high-purity strontium fluoride to raw material is relatively high, and current high-purity strontium fluoride raw material is mostly using high-purity
Strontium hydroxide or high-purity strontium carbonate are reacted with hydrofluoric acid, first prepare strontium fluoride slurry, then slurry is carried out dries pulverizing to get fluorine
Change strontium product；Containing for metal impurities ion in raw material can be effectively reduced by purifying to strontium chloride and sodium carbonate in somebody
Amount, then the raw material after purification is subjected to hybrid reaction and prepares basic carbonate strontium, basic carbonate strontium is reacted with hydrofluoric acid to be produced
High-purity strontium fluoride.
However, strontium hydroxide, strontium carbonate or strontium chloride no matter is used to do raw material, is reacted and lived by raw material in reaction process
The influence of property, reaction rate, the new solid phase strontium fluoride of generation can always form precipitating on solid material, thus to reactant into
Row cladding, influences the reactivity of raw material.In the system that solid-liquid reaction generates new solid phase, although cladding phenomenon can be reduced,
The requirement that high-purity strontium fluoride is not less than 99.9% is not achieved in the strontium fluoride for being difficult to avoid that, thus preparing always；And liquid phase synthesis is anti-
The strontium fluoride particle that should be generated is thin, causes product to be difficult to filtration washing, increases impurity content, it is difficult to realize industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method for preparing high-purity strontium fluoride in ethanol system,
It can overcome drawbacks described above of the existing technology, have impurity content low, and product purity is high, and production cost is low and economical
The advantages that high efficiency.
The present invention is implemented as follows:
A method of preparing high-purity strontium fluoride in ethanol system, it is characterised in that: the following steps are included:
(1) prepared by strontium chloride solution: strontium chloride is dissolved in the volume ratio of ethyl alcohol and water with 30~50wt% of mass concentration
To obtain strontium chloride solution in 0.7~1.2: 1 mixed solution；
(2) crystallization reaction: strontium fluoride crystal seed is added into strontium chloride solution obtained by step (1) under stiring, is added dropwise simultaneously
Ammonium fluoride solution is stirred for reacting, obtains suspension after charging；Wherein, strontium fluoride: strontium chloride: the molar ratio of ammonium fluoride is
0.15~0.3: 0.35~0.50: 1, the mass concentration of the ammonium fluoride solution is 10~30wt%；
(3) it is filtered, washed: suspension obtained by step (2) is filtered, reusable heat water washing, filtering obtain strontium fluoride filter
Cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is dried, then at 400~500 DEG C, calcination 3~
4h crushes firing product, obtains high-purity strontium fluoride powder.It is to guarantee in strontium fluoride that the calcination temperature, which selects 400~500 DEG C,
The ammonium chloride impurities of remaining can sufficiently volatilize.
Further, in step (2), the partial size of the strontium fluoride crystal seed is 100~200 mesh.If strontium fluoride particle is excessively thick,
Activity of crystal seed is insufficient, be unfavorable for it is fine grain grow up, if strontium fluoride particle is meticulous, wash poor filtration effect.
Further, in step (2), the feed time that ammonium fluoride solution is added dropwise is 0.5~1.5h, after charging
It is stirred for 1~1.5h of reaction.If charging rate is too fast, the strontium fluoride particle of generation is thin, washing filtering is not easy to, if charging rate
It crosses slowly, will increase corresponding production cost.
Further, in step (2), the speed of the stirring is 200~300r/min.
Further, in step (3), the temperature of the hot water is 65~95 DEG C.
Further, in step (3), the temperature of the hot water is 75~85 DEG C.It is washed using hot water, filter cake can be improved
Washing effect reduces wash water dosage；It is described to be filtered into vacuum filter.
Further, in step (4), the temperature of the drying is 90~125 DEG C, and the time of drying is 3~4h.
Further, in step (1), the strontium chloride is with 35~45wt% of mass concentration dissolution.
Further, in step 2), the strontium fluoride: strontium chloride: the molar ratio of ammonium fluoride be 0.2~0.25: 0.40~
0.45:1；The mass concentration of the ammonium fluoride solution is 20~25wt%.Ammonium fluoride is added with excessive proportion, guarantees chlorine
Changing strontium can react completely；Ammonium fluoride, strontium chloride solution the mass concentration saturated solution all close under room temperature, to guarantee filling for raw material
Divide dissolution, while reducing system amount of water as far as possible.
The present invention has the advantage that
The method of the present invention under the action of strontium fluoride crystal seed, is crystallized by induction using ammonium fluoride and strontium chloride as raw material
Principle makes fine grained strontium fluoride heterogeneous nucleation grow up, to avoid strontium fluoride plastic phenomenon, while in the solution using ethyl alcohol
Peptizaiton, the dispersion performance of enhancing strontium fluoride precipitating, so that the washing strainability of strontium fluoride is improved, remaining pair in product
Product ammonium chloride and impure alcohol can be removed by way of high temperature sintering, and prepared high-purity strontium fluoride product master contains
Amount >=99.9%, other impurities ion concentration can meet the requirement of optical grade material.
High-purity strontium fluoride is prepared using the method for the present invention, solves that strontium fluoride particle in traditional preparation methods is thin, sad filter
The problem of；And since the method for the present invention is reacted using excessive ammonium fluoride, ammonium fluoride and strontium chloride can realize it is complete react, only
There are a small amount of mechanical losses, and in terms of strontium element, strontium fluoride yield >=96% avoids the wasting of resources, reduce production cost, tool
There is good economic benefit.
Specific embodiment
The method that the present invention relates to a kind of to prepare high-purity strontium fluoride in ethanol system, it is characterised in that: including following step
It is rapid:
(1) prepared by strontium chloride solution: strontium chloride is dissolved in the volume ratio of ethyl alcohol and water with 30~50wt% of mass concentration
To obtain strontium chloride solution in 0.7~1.2: 1 mixed solution；
(2) crystallization reaction: strontium fluoride crystal seed is added into strontium chloride solution obtained by step (1) under stiring, is added dropwise simultaneously
Ammonium fluoride solution is stirred for reacting, obtains suspension after charging；Wherein, strontium fluoride: strontium chloride: the molar ratio of ammonium fluoride is
0.15~0.3: 0.35~0.50: 1, the mass concentration of the ammonium fluoride solution is 10~30wt%；
(3) it is filtered, washed: suspension obtained by step (2) is filtered, reusable heat water washing, filtering obtain strontium fluoride filter
Cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is dried, then at 400~500 DEG C, calcination 3~
4h crushes firing product, obtains high-purity strontium fluoride powder.It is to guarantee in strontium fluoride that the calcination temperature, which selects 400~500 DEG C,
The ammonium chloride impurities of remaining can sufficiently volatilize.
In step (2), the partial size of the strontium fluoride crystal seed is 100~200 mesh.If strontium fluoride particle is excessively thick, activity of crystal seed
Deficiency, be unfavorable for it is fine grain grow up, if strontium fluoride particle is meticulous, wash poor filtration effect.
In step (2), the feed time that ammonium fluoride solution is added dropwise is 0.5~1.5h, is stirred for after charging anti-
Answer 1~1.5h.If charging rate is too fast, the strontium fluoride particle of generation is thin, is not easy to washing filtering, if charging rate is excessively slow, meeting
Increase corresponding production cost.
In step (2), the speed of the stirring is 200~300r/min.
In step (3), the temperature of the hot water is 65~95 DEG C.
Preferably, in step (3), the temperature of the hot water is 75~85 DEG C.It is washed using hot water, washing for filter cake can be improved
Effect is washed, wash water dosage is reduced；It is described to be filtered into vacuum filter.
In step (4), the temperature of the drying is 90~125 DEG C, and the time of drying is 3~4h.
In step (1), the strontium chloride is with 35~45wt% of mass concentration dissolution.
In step (2), the strontium fluoride: strontium chloride: the molar ratio of ammonium fluoride is 0.2~0.25: 0.40~0.45: 1；Institute
The mass concentration for stating ammonium fluoride solution is 20~25wt%.Ammonium fluoride is added with excessive proportion, guarantees that strontium chloride can
Reaction completely；Ammonium fluoride, strontium chloride solution the mass concentration saturated solution all close under room temperature, to guarantee the abundant dissolution of raw material,
Reduce system amount of water as far as possible simultaneously.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
(1) prepared by strontium chloride solution: weighing 55.5g (0.35mol) anhydrous strontium chloride and being added to 103.1g volume ratio is 1: 1
Alcohol-water mixed solution in, stirring and dissolving obtains the strontium chloride solution of mass concentration 35wt%；
(2) 12.6g (0.1mol) strontium fluoride crystal seed (partial size crystallization reaction: is added in the strontium chloride solution obtained by step (1)
For 200~160 mesh), while the ammonium fluoride solution (ammonium fluoride content 1mol) of 246.7g mass concentration 15wt% is added dropwise, control is stirred
Speed 200r/min, feed time 0.5h are mixed, is further continued for being stirred to react 1h after charging, obtains suspension；
(3) it is filtered, washed: suspension obtained by step (2) being subjected to vacuum filter, then is washed with 65 DEG C of 1L of hot water
It washs, filter, obtain strontium fluoride filter cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is placed in baking oven, at 100 DEG C, is dried 4h, is then shifted
Into Muffle furnace, at 400 DEG C, calcination 3.5h crushes firing product, obtains high-purity strontium fluoride powder of 55.1g purity 99.91%,
Yield is 96.8%.
Embodiment 2
(1) prepared by strontium chloride solution: weighing 63.4g (0.4mol) anhydrous strontium chloride and being added to 95.1g volume ratio is 1: 1
In alcohol-water mixed solution, stirring and dissolving obtains the strontium chloride solution of mass concentration 40wt%；
(2) 25.2g (0.2mol) strontium fluoride crystal seed (partial size crystallization reaction: is added in the strontium chloride solution obtained by step (1)
For 160~140 mesh), while the ammonium fluoride solution (ammonium fluoride content lmol) of 185.0g mass concentration 20wt% is added dropwise, control is stirred
Speed 250r/min, feed time 0.5h are mixed, is further continued for being stirred to react 1h after charging, obtains suspension；
(3) it is filtered, washed: suspension obtained by step (2) being subjected to vacuum filter, then is washed with 70 DEG C of 1L of hot water
It washs, filter, obtain strontium fluoride filter cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is placed in baking oven, at 105 DEG C, is dried 3.5h, is then turned
It moves in Muffle furnace, at 450 DEG C, calcination 4h crushes firing product, obtains high-purity strontium fluoride powder of 74.0g purity 99.93%,
Yield is 97.1%.
Embodiment 3
(1) prepared by strontium chloride solution: weighing 71.4g (0.45mol) anhydrous strontium chloride and being added to 87.3g volume ratio is 1: 1
Alcohol-water mixed solution in, stirring and dissolving, obtain mass concentration be 45wt% strontium chloride solution；
(2) 31.4g (0.25mol) strontium fluoride crystal seed (grain crystallization reaction: is added in the strontium chloride solution obtained by step (1)
Diameter is 120~140 mesh), while the ammonium fluoride solution (ammonium fluoride content 1mol) of 148.0g mass concentration 25wt% is added dropwise, it controls
Mixing speed 300r/min, feed time 1.5h are further continued for being stirred to react 1h after charging, obtain suspension；
(3) it is filtered, washed: suspension obtained by step (2) being subjected to vacuum filter, then is washed with 80 DEG C of 1L of hot water
It washs, filter, obtain strontium fluoride filter cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is placed in baking oven, at 115 DEG C, is dried 3h, is then shifted
Into Muffle furnace, at 480 DEG C, calcination 3h crushes firing product, obtains high-purity strontium fluoride powder of 85.8g purity 99.95%, obtain
Rate is 96.2%.
Embodiment 4
(1) prepared by strontium chloride solution: weighing 76.1g (0.48mol) anhydrous strontium chloride and being added to 177.6g volume ratio is 1: 1
Alcohol-water mixed solution in, stirring and dissolving, obtain mass concentration be 30wt% strontium chloride solution；
(2) 37.7g (0.3mol) strontium fluoride crystal seed (partial size crystallization reaction: is added in the strontium chloride solution obtained by step (1)
For 100~120 mesh), while the ammonium fluoride solution (ammonium fluoride content 1mol) of 123.3g mass concentration 30wt% is added dropwise, control is stirred
Speed 280r/min, feed time 1h are mixed, is further continued for being stirred to react 1.5h after charging, obtains suspension；
(3) it is filtered, washed: suspension obtained by step (2) being subjected to vacuum filter, then is washed with 1L90 DEG C of hot water
It washs, filter, obtain strontium fluoride filter cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is placed in baking oven, at 125 DEG C, is dried 3h, is then shifted
Into Muffle furnace, at 500 DEG C, calcination 3h crushes firing product, obtains high-purity strontium fluoride powder of 96.2g purity 99.92%, obtain
Rate is 97.1%.
Principle components analysis is carried out to high-purity strontium fluoride product obtained by Examples 1 to 4, as shown in table 1.
High-purity strontium fluoride product Principle components analysis result obtained by 1 Examples 1 to 4 of table
Note: for high-purity strontium fluoride at present there is no national standard or professional standard, the standard in table 1 is the quality of enterprises
Standard, be it is prepared according to customer requirement, can satisfy the product of the standard can be used as optical glass material after client is on probation
The raw material of material and optical crystal.
In summary, the method for the present invention under the action of strontium fluoride crystal seed, is passed through using ammonium fluoride and strontium chloride as raw material
Crystallization principle is induced, fine grained strontium fluoride heterogeneous nucleation is made to grow up, to avoid strontium fluoride plastic phenomenon, while being existed using ethyl alcohol
Peptizaiton in solution, the dispersion performance of enhancing strontium fluoride precipitating, so that the washing strainability of strontium fluoride is improved, in product
Remaining by-product ammonium chloride and impure alcohol can be removed by way of high temperature sintering, prepared high-purity strontium fluoride
Main content >=99.9% of product, other impurities ion concentration can meet the requirement of optical grade material.
High-purity strontium fluoride is prepared using the method for the present invention, solves that strontium fluoride particle in traditional preparation methods is thin, sad filter
The problem of；And since the method for the present invention is reacted using excessive ammonium fluoride, ammonium fluoride and strontium chloride can realize it is complete react, only
There are a small amount of mechanical losses, and in terms of strontium element, strontium fluoride yield >=96% avoids the wasting of resources, reduce production cost, tool
There is good economic benefit.
Although specific embodiments of the present invention have been described above, those familiar with the art should be managed
Solution, we are merely exemplary described specific embodiment, rather than for the restriction to the scope of the present invention, it is familiar with this
The technical staff in field should be covered of the invention according to modification and variation equivalent made by spirit of the invention
In scope of the claimed protection.
Claims (9)
1. a kind of method for preparing high-purity strontium fluoride in ethanol system, it is characterised in that: the following steps are included:
(1) prepared by strontium chloride solution: strontium chloride is dissolved in the volume ratio of ethyl alcohol and water with 30~50wt% of mass concentration as 0.7
In~1.2: 1 mixed solution, strontium chloride solution is obtained；
(2) crystallization reaction: strontium fluoride crystal seed is added into strontium chloride solution obtained by step (1) under stiring, while fluorination is added dropwise
Ammonium salt solution is stirred for reacting, obtains suspension after charging；Wherein, strontium fluoride: strontium chloride: the molar ratio of ammonium fluoride is 0.15
~0.3: 0.35~0.50: 1, the mass concentration of the ammonium fluoride solution is 10~30wt%；
(3) it is filtered, washed: suspension obtained by step (2) is filtered, reusable heat water washing, filtering obtain strontium fluoride filter cake；
(4) drying, calcination: strontium fluoride filter cake obtained by step (3) is dried, then at 400~500 DEG C, 3~4h of calcination,
Firing product is crushed, high-purity strontium fluoride powder is obtained.
2. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1, it is characterised in that: step
(2) in, the partial size of the strontium fluoride crystal seed is 100~200 mesh.
3. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1 or 2, it is characterised in that:
In step (2), it is described be added dropwise ammonium fluoride solution feed time be 0.5~1.5h, be stirred for after charging reaction 1~
1.5h。
4. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1 or 2, it is characterised in that:
In step (2), the speed of the stirring is 200~300r/min.
5. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1 or 2, it is characterised in that:
In step (3), the temperature of the hot water is 65~95 DEG C.
6. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 5, it is characterised in that: step
(3) in, the temperature of the hot water is 75~85 DEG C.
7. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1 or 2, it is characterised in that:
In step (4), the temperature of the drying is 90~125 DEG C, and the time of drying is 3~4h.
8. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1 or 2, it is characterised in that:
In step (1), the strontium chloride is with 35~45wt% of mass concentration dissolution.
9. a kind of method for preparing high-purity strontium fluoride in ethanol system according to claim 1 or 2, it is characterised in that:
In step (2), the strontium fluoride: strontium chloride: the molar ratio of ammonium fluoride is 0.2~0.25: 0.40~0.45: 1；The ammonium fluoride
The mass concentration of solution is 20~25wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180612A (en) * | 2021-12-09 | 2022-03-15 | 安徽光智科技有限公司 | Preparation method of high-purity barium fluoride of optical material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104773749A (en) * | 2015-04-10 | 2015-07-15 | 湖南有色氟化学科技发展有限公司 | Method for preparing high-purity calcium fluoride in ethanol system |
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2018
- 2018-09-19 CN CN201811093150.6A patent/CN108946782A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104773749A (en) * | 2015-04-10 | 2015-07-15 | 湖南有色氟化学科技发展有限公司 | Method for preparing high-purity calcium fluoride in ethanol system |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180612A (en) * | 2021-12-09 | 2022-03-15 | 安徽光智科技有限公司 | Preparation method of high-purity barium fluoride of optical material |
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