CN107381613A - A kind of synthetic method of single phase cubic body fluorite - Google Patents
A kind of synthetic method of single phase cubic body fluorite Download PDFInfo
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- CN107381613A CN107381613A CN201710732466.4A CN201710732466A CN107381613A CN 107381613 A CN107381613 A CN 107381613A CN 201710732466 A CN201710732466 A CN 201710732466A CN 107381613 A CN107381613 A CN 107381613A
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of single phase cubic body fluorite, comprise the following steps：Step 1：At normal temperatures, soluble fluoride and soluble calcium salt are configured to the solution of certain mole of solubility with deionized water；Step 2：Enuatrol or lauryl sodium sulfate are dissolved in soluble fluoride solution according to a certain percentage；Step 3：Control soluble calcium salt respectively using peristaltic pump and dissolved the addition flow of the soluble fluoride of enuatrol, certain power ultrasonic processing mixed solution certain time is used when controlling flow, it is reacted under ultrasonication；Step 4：Mixed solution product after supersound process is continued into mechanical agitation certain time, continues to react, then is aged certain time, obtains reaction precipitate；Step 5：Fluorite can be obtained after the reaction precipitate that step 4 obtains is filtered, washed and dried.Single phase cubic body fluorite good dispersion prepared by the present invention, avoids agglomeration.
Description
Technical field
The invention belongs to inorganic compound and mineral preparing technical field, and in particular to a kind of conjunction of single phase cubic body fluorite
Into method.
Background technology
Fluorite is a kind of excellent optical material, has good chemical stability and optical clarity.Calcirm-fluoride it is saturating
Optical range is wide, and from deep ultraviolet until near-infrared (0.125~10 μm), low phonon energy can suppress the noradiative transition of electronics
Move, therefore be especially suitable for doing the matrix material of various optics and solid state laser.
Fluorite is to apply and study very extensive alkali earth metal fluoride, there is superior optical property, can the company of being used as
The cushion of semiconductor is connect, and has good F-Ionic conductivity.CaF2It is the F- ionic conduction Journal of Sex Research for carrying out nano fluoride
Main material, at present the method for synthetising nanometre powder body mainly have：1) chemical vapour deposition technique；2) vapor condensation method；3) colloidal sol
Gel method；4) microemulsion method；5) hydro-thermal method etc..
The minimum 60nm of average grain diameter CaF has been made with microemulsion method for stone Chun-shan Mountain etc.2Nano-powder, Li Yadong etc. are with first
The method of precipitation and then hydro-thermal process is prepared for CaF2, obtain the precipitation that particle diameter is more than 100 nanometers, grain prepared by two methods
Footpath is relatively large.S.tark is prepared for CaF with flame method2Etc. a variety of alkali earth metal fluoride nano-powders.Ye Jin etc. are used
CTAB/ water/hexamethylene/n-amyl alcohol microemulsion system is prepared for SrF2:Eu3+ nano-powders.Aubry P and Bensalah A etc. is used
Reverse microemulsion process has synthesized CaF of the average grain diameter in 20nm or so2Nano-powder.Wang Jianshe etc. use formaldehyde conduct
Solvent has synthesized Eu3+, Tb3+ doping CaF2Nanocrystal.
The problems such as fluorite prepared by existing method is mostly spherical, and characteristic parameter is difficult to meet industrial requirement, and production technology
Complexity, condition are harsh, it is difficult to industrialized production and application.There is presently no mild condition, workable, favorable repeatability system
The maturation method of standby cube fluorite.
The content of the invention
The invention aims to the technical problem for solving the preparation of cube fluorite and easily assembling, and provide a kind of single-phase
The preparation method of cube fluorite.
The present invention is for cube fluorite synthesis technique is complicated, condition is harsh, production cost is high, is mostly the skills such as spheric granules
Deficiency in art, it is proposed that one kind is synthesized vertical using soluble fluoride and soluble calcium salt as raw material using ultrasonic chemical process
The method of cube fluorite.It is synthesis technique simple possible, green, there is preferable environmental benefit and economic benefit.
To reach above-mentioned technique effect, the present invention provides following technical scheme, comprised the following steps that：
A kind of preparation method of single phase cubic body fluorite, comprises the following steps：
Step 1：At normal temperatures, with deionized water by soluble fluoride and soluble calcium salt be configured to certain mole it is molten
The solution of degree；
Step 2：Enuatrol or lauryl sodium sulfate are dissolved in soluble fluoride solution according to a certain percentage；
Step 3：Control soluble calcium salt respectively using peristaltic pump and dissolve the addition of the soluble fluoride of enuatrol
Flow, certain power ultrasonic processing mixed solution certain time is used when controlling flow, it is carried out under ultrasonication instead
Should；
Step 4：Mixed solution product after supersound process is continued into mechanical agitation certain time, continues to react, then
Certain time is aged, obtains reaction precipitate；
Step 5：Fluorite can be obtained after the reaction precipitate that step 4 obtains is filtered, washed and dried.
By such scheme, the soluble fluoride described in step 1 is：Sodium fluoride, potassium fluoride and ammonium fluoride etc.；It is solvable
Property calcium salt is：Calcium chloride and calcium nitrate, certain mole of solubility are：Sodium fluoride, potassium fluoride, ammonium fluoride, calcium chloride and calcium nitrate are
0.1mol/L-1.0mol/L, mole solubility of fluorine ion are 2 times of calcium ion mole solubility；
By such scheme, enuatrol or lauryl sodium sulfate described in step 2 are according to a certain percentage：0.1%-
The quality percentage solubility of 6%wt fluorine.
By such scheme, described in step 3 is with certain power while in coutroi velocity：500-1800w, ultrasonic wave
Processing mixed solution certain time is 10min-60min；Soluble calcium salt and soluble carbonate salt are controlled using peristaltic pump respectively
Flow be 6ml/min-60ml/min；With ultrasonication mixed solution certain time it is 1min- while in coutroi velocity
30min；
By such scheme, the mechanical agitation certain time described in step 4 is：10min-180min；
By such scheme, the certain time that is aged again described in step 4 is：10min-60min；
The beneficial effects of the present invention are：1), the flow of the invention by controlling soluble calcium salt and soluble fluoride,
Adding simultaneously has peptizaiton, the enuatrol of chelation and lauryl sodium sulfate, obtains fluorite crystals stable abundant
Growth, avoid agglomeration.The pattern of control fluorite is can be very good simultaneously, obtains the fluorite of single phase cubic bodily form looks, and
And its characteristic parameter is homogeneous, purity is high.2) present invention process flow is short, green, environmental benefit and remarkable in economical benefits, fits
Close large-scale industrial production.
Brief description of the drawings
The XRD of fluorite prepared by Fig. 1 embodiment of the present invention 1；
The SEM figures of fluorite prepared by Fig. 2 embodiment of the present invention 1；
The XRD of fluorite prepared by Fig. 3 embodiment of the present invention 2；
The SEM figures of fluorite prepared by Fig. 4 embodiment of the present invention 2；
The XRD of fluorite prepared by Fig. 5 embodiment of the present invention 3；
The SEM figures of fluorite prepared by Fig. 6 embodiment of the present invention 5；
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
At normal temperatures, with ultra-pure water compound concentration is 0.8mol/L respectively NaF and 0.4mol/LCa (NO3)2Solution, will
1%wt enuatrol is dissolved into Fluorinse, controls NaF solution and Ca (NO respectively with peristaltic pump3)2The flow of solution adds
Enter into reactor, carried out in the reactor in coutroi velocity ultrasonication certain time, the flow of two kinds of solution is
6ml/min, ultrasonic treatment time 17.5min, operating power 900w, after ultrasonication stops, subsequent solution is with same
Flow is added in reactor, until all add, then with 10min is aged again after magnetic stirrer 2h, by reaction product mistake
Filter, with milli-Q water repeatedly to neutrality, sediment is put into air dry oven and dried, drying temperature is 100 DEG C, drying time
12h, finally obtain required product.
Fig. 3 is the XRD of the product synthesized by the present embodiment, and as seen from the figure, the θ of the angle of diffraction 2 is located at the θ of the angle of diffraction 2 and is located at
28.36 °, 47.08 °, 55.86 °, 68.76 °, 75.92 ° there is obvious diffraction maximum, this and fluorite standard Pdf cards
(NO.77-2094) data result is consistent.Occur in figure without miscellaneous peak, show to synthesize fluorite purity height.Peak height and sharp, it is shown that
Fluorite crystallinity is good.
Fig. 4 is that the SEM of product prepared by the present embodiment schemes, and fluorite is cube as seen from the figure, and the cube length of side is 100-
300nm, although crystal size is not very uniformly, good dispersion, plane of crystal is smooth, few surface defects, illustrates fluorite crystals
Grow sufficiently complete.
Embodiment 2
At normal temperatures, with the ultra-pure water NaF and 0.4mol/L Ca (NO that compound concentration is 0.8mol/L respectively3)2Solution, will
1%wt lauryl sodium sulfate is dissolved into Fluorinse, controls NaF solution and Ca (NO respectively with peristaltic pump3)2Solution
Flow be added in reactor, carried out in the reactor in coutroi velocity ultrasonication certain time, two kinds of solution
Flow is 6ml/min, ultrasonic treatment time 17.5min, operating power 900w.After ultrasonication stops, subsequent solution
Added in reactor with same flow, until all adding, then with 10min is aged again after magnetic stirrer 2h, will reacted
Product filters, and with milli-Q water repeatedly to neutrality, sediment is put into air dry oven and dried, drying temperature is 100 DEG C, is done
Dry time 12h, finally obtains required product.
Fig. 3 be the present embodiment synthesized by product XRD, as seen from the figure, the θ of the angle of diffraction 2 positioned at 28.36 °, 47.08 °,
55.86 °, 68.76 °, 75.92 ° nearby there is obvious diffraction maximum, and this and fluorite standard Pdf cards (NO.77-2094) count
It is consistent according to result.Occur without miscellaneous peak, show fluorite purity height, peak height and sharp, it is shown that fluorite crystallinity is good.
Fig. 4 is that the SEM of product prepared by the present embodiment schemes, and fluorite is cube as seen from the figure, and the cube length of side is 50-
500nm, crystal size is uneven, but good dispersion, and plane of crystal is smooth, few surface defects, and fluorite crystals growth is abundant.
Embodiment 3
At normal temperatures, with the ultra-pure water NaF and 0.4mol/L Ca (NO that compound concentration is 0.8mol/L respectively3)2Solution, will
5%wt enuatrol is dissolved into Fluorinse, controls NaF solution and Ca (NO respectively with peristaltic pump3)2The flow of solution adds
Enter into reactor, carried out in the reactor in coutroi velocity ultrasonication certain time, the flow of two kinds of solution is
3ml/min, ultrasonic treatment time 34min, operating power 600w.After ultrasonication stops, subsequent solution is equally to flow
Amount is added in reactor, until all adding, then with 10min is aged again after magnetic stirrer 2h, reaction product is filtered,
With milli-Q water repeatedly to neutrality, sediment is put into air dry oven and dried, drying temperature is 100 DEG C, drying time
12h, finally obtain required product.
Embodiment 4
At normal temperatures, with the ultra-pure water NaF and 0.1mol/L Ca (NO that compound concentration is 0.2mol/L respectively3)2Solution, will
3%wt lauryl sodium sulfate is dissolved into Fluorinse, controls NaF solution and Ca (NO respectively with peristaltic pump3)2Solution
Flow be added in reactor, carried out in the reactor in coutroi velocity ultrasonication certain time, two kinds of solution
Flow is 12ml/min, ultrasonic treatment time 18min, operating power 1800w.After ultrasonication stops, subsequent solution
Added in reactor with same flow, until all adding, then with 10min is aged again after magnetic stirrer 2h, will reacted
Product filters, and with milli-Q water repeatedly to neutrality, sediment is put into air dry oven and dried, drying temperature is 100 DEG C, is done
Dry time 12h, finally obtains required product.
Embodiment 5
At normal temperatures, with the ultra-pure water KF and 0.5mol/L Ca (NO that compound concentration is 1.0mol/L respectively3)2Solution, will
6%wt enuatrol is dissolved into potassium fluoride solution, controls KF solution and Ca (NO respectively with peristaltic pump3)2The flow of solution adds
Into reactor, carried out in the reactor in coutroi velocity ultrasonication certain time, the flow of two kinds of solution is 3ml/
Min, ultrasonic treatment time 50min, operating power 500w.After ultrasonication stops, subsequent solution is added with same flow
Enter in reactor, until all adding, then with 20min is aged again after magnetic stirrer 2h, reaction product is filtered, with super
Sediment repeatedly to neutrality, is put into air dry oven and dried, drying temperature is 100 DEG C, drying time 12h, most by pure water
Required product is obtained eventually.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (6)
1. a kind of preparation method of single phase cubic body fluorite, it is characterised in that comprise the following steps：
Step 1：At normal temperatures, soluble fluoride and soluble calcium salt are configured to certain mole of solubility with deionized water
Solution；
Step 2：Enuatrol or lauryl sodium sulfate are dissolved in soluble fluoride solution according to a certain percentage；
Step 3：Control soluble calcium salt respectively using peristaltic pump and dissolve the addition stream of the soluble fluoride of enuatrol
Amount, certain power ultrasonic processing mixed solution certain time is used when controlling flow, it is reacted under ultrasonication；
Step 4：Mixed solution product after supersound process is continued into mechanical agitation certain time, continues to react, then be aged
Certain time, obtain reaction precipitate；
Step 5：Fluorite can be obtained after the reaction precipitate that step 4 obtains is filtered, washed and dried.
2. the preparation method of single phase cubic body fluorite according to claim 1, it is characterised in that described in step 1 can
Dissolubility fluoride is：Sodium fluoride, potassium fluoride and ammonium fluoride；Soluble calcium salt is：Calcium chloride and calcium nitrate, certain mole of solubility
For：Sodium fluoride, potassium fluoride, ammonium fluoride, calcium chloride and calcium nitrate are 0.1mol/L-1.0mol/L, and mole solubility of fluorine ion is
2 times of calcium ion mole solubility.
3. the preparation method of single phase cubic body fluorite according to claim 1, it is characterised in that the oil described in step 2
Sour sodium or lauryl sodium sulfate are according to a certain percentage：The quality percentage solubility of 0.1%-6%wt fluorine.
4. the preparation method of single phase cubic body fluorite according to claim 1, it is characterised in that described in step 3
It is with certain power in coutroi velocity：500-1800w, ultrasonication mixed solution certain time are 10min-60min；Adopt
It is 6ml/min-60ml/min to control the flow of soluble calcium salt and soluble carbonate salt respectively with peristaltic pump；In side coutroi velocity
While it is 1min-30min with ultrasonication mixed solution certain time.
5. the preparation method of single phase cubic body fluorite according to claim 1, it is characterised in that the machine described in step 4
Tool stirring certain time be：10min-180min.
6. the preparation method of single phase cubic body fluorite according to claim 1, it is characterised in that described in step 4 again
Ageing certain time be：10min-60min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2349147A (en) * | 1999-04-19 | 2000-10-25 | Univ Sheffield | Doped calcium fluoride precipitate |
| JP2009057250A (en) * | 2007-08-31 | 2009-03-19 | Univ Of Tokyo | Purification method of fluorite |
| CN101885505A (en) * | 2010-08-18 | 2010-11-17 | 中国科学院长春应用化学研究所 | Method for preparing calcium fluoride hollow nanospheres |
| CN102583486A (en) * | 2012-03-09 | 2012-07-18 | 山东轻工业学院 | Preparation method of nano calcium fluoride for self-lubricating tool material |
-
2017
- 2017-08-24 CN CN201710732466.4A patent/CN107381613B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2349147A (en) * | 1999-04-19 | 2000-10-25 | Univ Sheffield | Doped calcium fluoride precipitate |
| JP2009057250A (en) * | 2007-08-31 | 2009-03-19 | Univ Of Tokyo | Purification method of fluorite |
| CN101885505A (en) * | 2010-08-18 | 2010-11-17 | 中国科学院长春应用化学研究所 | Method for preparing calcium fluoride hollow nanospheres |
| CN102583486A (en) * | 2012-03-09 | 2012-07-18 | 山东轻工业学院 | Preparation method of nano calcium fluoride for self-lubricating tool material |
Non-Patent Citations (1)
| Title |
|---|
| 王淼等: ""超声化学法制备不同形貌的CaF2微米晶"", 《无机化学学报》 * |
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