CN104071814B - Preparation method of magnesium fluoride with high specific surface area - Google Patents
Preparation method of magnesium fluoride with high specific surface area Download PDFInfo
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Abstract
The invention discloses a preparation method of magnesium fluoride with high specific surface area. The preparation method comprises the steps of: mixing a magnesium source water solution with a fluorine source water solution, wherein the obtained mixed solution contains a carbon source, the carbon source is one of or a mixture of several of saccharose, glucose, furfuryl alcohol, P123, polyvinyl alcohol and phenolic resin and the mole ratio of the carbon source to the magnesium source is 1-10: 1 based on C to Mg; stirring for full reaction and standing for ageing and removing moisture to obtain a carbon source-containing magnesium fluoride precursor; carrying out pre-carbonization on the carbon source-containing magnesium fluoride precursor and then carrying out carbonization in an inert atmosphere to obtain carbon-doped magnesium fluoride; finally carrying out high-temperature decarburization in an oxygen-bearing atmosphere to obtain the magnesium fluoride product. The preparation method is simple, low in production cost, small in environmental pressure, easy to operate and control and low in device corrosion, and has favorable economical, environmental and social benefits.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium fluoride, particularly relate to a kind of preparation method of high-specific surface area magnesium fluoride.
Technical background
Magnesium fluoride is starting material important in industrial production, is widely used in pottery, glass manufacture; Fusing assistant is made in metallurgical industry; Making coatings, mould material or fluorescent material in optics.Especially hot pressing magnesium fluoride material, because it has high infrared transmittivity at medium-wave infrared wave band; Higher physical strength and thermal-shock resistance; Less specific inductivity and the various features such as dielectric loss and isotropy, be good medium-wave infrared window, dome material and medium-wave infrared/millimeter wave (microwave) combined antenna cover material, be widely used in infrared track, detection, the guidance systems such as infrared guidance, infrared imaging guidance, Infrared/Millimeter Waves (microwave) combined guidance and aircraft Infrared pod, electro-optic radar.Magnesium fluoride has the features such as extraordinary erosion resistance, high stability simultaneously, can as catalyzer or carrier for having in the catalyzed reaction of particular surroundings, such as, as contained the hydrofluoric reaction of corrosive gases, the solid acid catalyst commonly used in the production process of fluorochlorohydrocarbon (CFCs), hydrogen fluorohydrocarbon (HCFCs).Usually exchange chloride for fluoride can be related in the process of current industrial production hydrogen fluorohydrocarbon and Chlorofluorocarbons (CFCs); conventional catalyzer is the chromium-based catalysts of aluminum fluoride load; but aluminium base solid acid catalyst acidity is stronger; easily coking in catalytic reaction process; make rapid catalyst deactivation, affect catalyst life.And magnesium fluoride as carrier Kaolinite Preparation of Catalyst time, there is the acid site of medium tenacity, there is better stability and work-ing life in exchange chloride for fluoride, therefore there is better application prospect.
Research shows that exchange chloride for fluoride is a typical acid catalyzed reaction, when magnesium fluoride is as fluorination catalyst agent carrier, the activity of its specific surface area and catalyzer is closely related, when the specific surface area of magnesium fluoride is higher, its degree of crystallinity is lower, magnesium ion on surface will exist with the form of polygamy position, and Lewis acidic site is more, and the number of active sites is more.So the meaning of synthesizing high specific surface area magnesium fluoride is very great.
At present, the document both at home and abroad about the preparation method of high-specific area nano magnesium fluoride is less, and domestic also do not have Patents.It is fluorine source that the Erhard Kemnitz of Germany's Humboldt University teaches with HF, in anhydrous conditions, adopts expensive organic-magnesium (Mg (OMe)
2), prepare micro-specific surface area at 150m with microwave-assisted sol-gel method
2the HS-MgF of/g
2crystal.Professor Wojciechowska etc. of Brussels,Belgium university mixes the magnesium oxide MgO of high-specific surface area in magnesium fluoride crystal, and with increasing specific surface area, the specific surface area of resulting materials can reach 126m
2/ g.Zelanian professors Wuttke etc. have prepared the MgF of hydroxyl with fluoridizing-being hydrolyzed two-step approach
2-x(OH)
x, then through the process of the steps such as roasting, can produce specific surface area is 120-150m
2the metal oxygen fluorochemical of/g.The production of industrial magnesium fluoride adopts hydrofluoric acid and magnesite powder to be prepared by the precipitator method as raw material usually, and other also have microemulsion method, sol-gel method and the microwave-assisted precipitator method etc.The MgF that the existing precipitator method are produced
2that degree of crystallinity is higher, and specific surface area is less (generally at 50m close to neutral solid matter
2below, some is only 5-10m
2).The Wu Wane of No.2 Artillery Engineering College, PLA etc. with magnesium chloride and Neutral ammonium fluoride for raw material, adopt direct precipitation method, in a nitrogen atmosphere, utilize the equipment such as condensation reflux unit, ultrasonic cleaner to obtain a kind of ball shaped nano magnesium fluoride particle, purity is higher.The Li Shijiang of Duo-fluoride Chemicals Co., Ltd. etc. are with silicofluoric acid and magnesium oxide for raw material, and after filtration, concentrated, washing, hydrolysis, drying and other steps obtain highly purified magnesium fluoride.The Li Zhonghuas of No.5 Academy, China Space Science and Technology Group Co., Ltd. etc. adopt magnetron sputtering method composition target to prepare ITO/MgF
2electroconductibility compound coating, its snappiness is good, has anti-reflection effect to light.Up to the present, the patent prepared about magnesium fluoride material mainly concentrates on the preparation of highly purified magnesium fluoride and its application on optical material and mould material, also there is no patent prepared by high-ratio surface magnesium fluoride, not using the patent of magnesium fluoride as support of the catalyst or solid acid catalyst yet.
In sum, the preparation method of the magnesium fluoride of existing high-specific surface area, at least there is one of following problem: (1) starting material are expensive: adopt expensive organic-magnesium source, 2) production or severe reaction conditions: react under the environment of anhydrous and oxygen-free, 3) technical process complexity: in roasting process, add appropriate pore-forming material.4) raw material has severe corrosive: have aggressive to experimental installation.So make high-ratio surface magnesium fluoride output little, difficulty is amplified in industry, is difficult to realize industrialization.
Summary of the invention
The object of the invention is the specific surface area of the magnesium fluoride prepared for existing most methods compared with low, complicated process of preparation, production cost is high, environmental protection pressure is large, be not easy to operation and controlling, the weak point large to corrosion of equipment, provide that a kind of preparation method is simple, production cost is low, environmental protection pressure is little, be easy to operate and control, the method for preparing high-specific surface area magnesium fluoride little to corrosion of equipment.
For achieving the above object, the technical solution used in the present invention is:
A kind of preparation method of magnesium fluoride, comprise: make the magnesium source aqueous solution and fluorine source aqueous solution, also containing carbon source in gained mixed solution, described carbon source is sucrose, glucose, furfuryl alcohol, P123, polyvinyl alcohol, the mixture of one or more in resol, the mol ratio in carbon source and magnesium source counts 1 ~ 10:1 with C:Mg, the magnesium fluoride presoma that aging removing moisture obtains carbonaceous sources is left standstill after stirring lower fully reaction, again by the pre-carbonization in oxygen-containing atmosphere of the magnesium fluoride presoma of carbonaceous sources, then carbonization obtains the magnesium fluoride of doping charcoal in an inert atmosphere, magnesium fluoride product is obtained finally by high temperature removal charcoal in oxygen-containing atmosphere.
In the present invention, the kind of carbon source and add-on have material impact for magnesium fluoride product structure, and the preferred carbon source of the present invention is sucrose.Carbon source can add with the form of solid or the aqueous solution, and it can first original position add in the magnesium source aqueous solution or the fluorine source aqueous solution, or directly adds in both mixed solution.
In the present invention, magnesium source adopts magnesium acetate, magnesium oxalate, magnesium nitrate, the mixture of one or more in magnesium chloride, preferred following a kind of or both mixture: magnesium acetate, magnesium oxalate.
In the present invention, fluorine source adopts the mixture of one or more in Neutral ammonium fluoride, Potassium monofluoride, Sodium Fluoride, is preferably Neutral ammonium fluoride.
In the present invention, the mol ratio in carbon source and magnesium source is preferably 3 ~ 6:1 in C:Mg, is more preferably 4:1.
In the present invention, the mol ratio in magnesium source and fluorine source is preferably 1:2 in Mg:F.
In the present invention, the reaction in fluorine source and magnesium source is carried out under the temperature condition of 20 ~ 80 DEG C, and the reaction times is 0.5 ~ 10 hour, is preferably 2 ~ 10 hours.
In the present invention, the pre-carbonization of the magnesium fluoride presoma of carbonaceous sources is carried out in oxygen-containing atmosphere, the preferred air atmosphere of described oxygen-containing atmosphere or oxygen-containing gas volume concentrations are the oxygen of 1 ~ 50% and the mixed atmosphere of nitrogen, described pre-charing is preferably carried out in the temperature range of 80 ~ 180 DEG C, pre-carbonization time preferably 5 ~ 20 hours.
In the present invention, described carbonization is carried out in an inert atmosphere, described inert atmosphere preferred nitrogen atmosphere or rare gas element (such as argon gas or helium) atmosphere; Described carbonization is preferably carried out under the temperature condition of 120 ~ 450 DEG C (more preferably 300 ~ 400 DEG C), and carbonization time preferably 1 ~ 10 hour, is more preferably 2 ~ 5 hours.
In the present invention, described " high temperature removal charcoal " carries out in oxygen-containing atmosphere, the preferred air atmosphere of described oxygen-containing atmosphere or oxygen-containing gas volume concentrations are the oxygen of 1 ~ 50% and the mixed atmosphere of nitrogen, and temperature of reaction preferably 250 ~ 500 DEG C, is more preferably 350 ~ 500 DEG C; Preferably 2 ~ 12 hours reaction times, more preferably 4 ~ 6 hours.
As preferably, the preparation method of magnesium fluoride of the present invention, carries out in accordance with the following steps:
(1) make the magnesium source aqueous solution and fluorine source aqueous solution, also containing carbon source in gained mixed solution, the mol ratio in carbon source and magnesium source counts 1 ~ 10:1 with C:Mg, in 20 ~ 80 DEG C of reactions 2 ~ 10 hours under stirring, stops stirring; Described carbon source adopts the mixture of one or more in sucrose, glucose, furfuryl alcohol, P123, polyvinyl alcohol, resol; Described magnesium source adopts the mixture of one or more in magnesium acetate, magnesium oxalate, magnesium nitrate, magnesium chloride; Described fluorine source adopts the mixture of one or more in Neutral ammonium fluoride, Potassium monofluoride, Sodium Fluoride;
(2) the reaction solution constant temperature that step (1) obtains is left standstill aging removing moisture, obtain the magnesium fluoride presoma of carbonaceous sources;
(3) the magnesium fluoride presoma of carbonaceous sources is first under an oxygen-containing atmosphere in 80 ~ 180 DEG C of charings 5 ~ 20 hours in advance, then carbonization 2-5 hour at 300 ~ 400 DEG C of temperature under an inert atmosphere, the magnesium fluoride of the charcoal that obtains adulterating;
(4) magnesium fluoride of doping charcoal is under an oxygen-containing atmosphere in 250 ~ 500 DEG C of roastings carbon removal in 2 ~ 12 hours, obtains magnesium fluoride product.
Compared with prior art, beneficial effect of the present invention is:
(1) the inventive method flow process is short, and equipment is simple, carries out in aqueous, is easy to control.
(2) industrial chemicals cheap and easy to get that the raw material selection reacted is common, has saved cost, has increased economic efficiency.
(3) in whole technological process, replace the hydrogen fluoride of severe corrosive, and non-corrosiveness product generates, and adopt water as solvent with the reactant fluorochemical of non-corrosiveness gentleness, solution is in neutral, and reaction conditions is gentle.
(4) magnesium fluoride that the present invention obtains has high-specific surface area.
(5) system of the present invention magnesium fluoride through pyroprocessing, generally specific surface will be caused to decline due to magnesium fluoride sintering when this temperature and following temperature use, thus cause the reduction of acidity of catalyst position and cause catalyst activity reduction.Therefore the gas-phase reaction that this material is adapted at below treatment temp uses as catalyzer or support of the catalyst.
To sum up, the present invention has good economic benefit, and environmental benefit and social benefit, be suitable for promotion and application.
Accompanying drawing explanation
Fig. 1 is the high-specific surface area magnesium fluoride nitrogen adsorption isotherm figure that embodiment 1 obtains.
Fig. 2 is the graph of pore diameter distribution of the high-specific surface area magnesium fluoride that embodiment 1 obtains.
Fig. 3 is the x ray diffration pattern x of the high-specific surface area magnesium fluoride that embodiment 1 obtains.
Specific examples mode
Below by some embodiments, high-specific surface area magnesium fluoride of the present invention is further described, but the present invention is not limited to these embodiments.
Embodiment 1
Prepare the NH of the isopyknic 2mol/L of each 100ml
4mg (the CH of F solution and 1mol/L
3cOO)
24H
2o solution, and in magnesium acetate solution, add sucrose (containing C 0.4mol), and sucrose is dissolved completely.Mixed by positive addition, and open magnetic agitation simultaneously, react 7 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 100 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 400 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, roasting 4 hours removing charcoal templates in last retort furnace under 400 DEG C of air atmospheres, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 184m
2/ g, pore volume is 0.35cc/g, and most probable pore size is distributed as 10.9nm.
The high-specific surface area magnesium fluoride nitrogen adsorption isotherm figure that this example obtains, graph of pore diameter distribution, X-ray diffractogram are respectively Fig. 1, Fig. 2 and Fig. 3.As can be seen from Figure 1, the method gained magnesium fluoride is IV type adsorption isothermal line, is the typical adsorption thermoisopleth type that mesopore material has.As can be seen from Figure 2, its pore size distribution is also comparatively concentrated.As can be seen from Figure 3, XRD figure is typical magnesium fluoride crystal phase structure.
Embodiment 2
Prepare the NaF solution of the isopyknic 2mol/L of each 100ml and the Mg (CH of 1mol/L
3cOO)
24H
2o solution, and in magnesium acetate solution, add sucrose (containing C 0.1mol), and sucrose is dissolved completely.Mixed by positive addition, and open magnetic agitation simultaneously, react 7 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 100 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 400 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, roasting 3 hours removing charcoal templates in last retort furnace under 400 DEG C of air atmospheres, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 73m
2/ g.
Embodiment 3
Prepare the NH of the isopyknic 2mol/L of each 100ml
4the MgC of F solution and 1 mol/L
2o
4.2H
2o solution, and in ammonium fluoride solution, add sucrose (containing C 1mol), and sucrose is dissolved completely.Mixed by anti-addition, and open magnetic agitation simultaneously, react 7 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 100 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 400 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, roasting 12 hours removing charcoal templates in last retort furnace under 400 DEG C of air atmospheres, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 153m
2/ g.
Embodiment 4
Prepare the NH of the isopyknic 2mol/L of each 100ml
4mg (the CH of F solution and 1mol/L
3cOO)
24H
2o solution, configure C concentration is that the sucrose solution 100ml of 2mol/L is as reaction end liquid simultaneously.Then fluorine source and magnesium source co-precipitation are joined in pre-configured sucrose solution, and open magnetic agitation simultaneously, react 2 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 80 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 350 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, roasting 6 hours removing charcoal templates in last retort furnace under 500 DEG C of air atmospheres, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 133m
2/ g.
Embodiment 5
Prepare the KF solution of the isopyknic 2mol/L of each 100ml and the Mg (NO of 1mol/L
3)
2solution, configure C concentration is that the sucrose solution 100ml of 6mol/L is as reaction end liquid simultaneously.Then fluorine source and magnesium source co-precipitation are joined in pre-configured sucrose solution, and open magnetic agitation simultaneously, react 2 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 80 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 350 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, roasting 2 hours removing charcoal templates in last retort furnace under 500 DEG C of oxygen atmospheres, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 103m
2/ g.
Embodiment 6
Prepare the NH of the isopyknic 2mol/L of each 100ml
4mg (the CH of F solution and 1 mol/L
3cOO)
24H
2o solution, and in magnesium acetate solution, add furfuryl alcohol (containing C 0.6mol), and furfuryl alcohol is dissolved completely.Mixed by anti-addition, and open magnetic agitation simultaneously, react 7 hours at the temperature of 80 DEG C, then constant temperature leaves standstill aging 3 hours and boils off upper strata moisture, in baking oven, 150 DEG C are spent the night, after pre-charing at 360 DEG C roasting carbonization 3h under argon gas atmosphere, obtain the magnesium fluoride containing charcoal.Magnesium fluoride containing charcoal is put into High Temperature Furnaces Heating Apparatus 350 DEG C of fluidizing air atmosphere and calcines 12h, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 203m
2/ g.
Embodiment 7
Prepare the NH of the isopyknic 1mol/L of each 100ml
4mg (the CH of F solution and 0.5mol/L
3cOO)
24H
2o solution, and P1234.0g is added in magnesium acetate solution, and P123 is dissolved completely.Mixed by anti-addition, and open magnetic agitation simultaneously, react 7 hours at the temperature of 80 DEG C, then constant temperature leaves standstill aging 3 hours and boils off upper strata moisture, in baking oven, 150 DEG C are spent the night, after pre-charing at 360 DEG C roasting carbonization 3h under argon gas atmosphere, obtain the magnesium fluoride containing charcoal.Magnesium fluoride containing charcoal is put into High Temperature Furnaces Heating Apparatus 350 DEG C of fluidizing air atmosphere and calcines 12h, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 146m
2/ g.
Embodiment 8
Prepare the NH of the isopyknic 2mol/L of each 100ml
4mg (the CH of F solution and 1mol/L
3cOO)
24H
2o solution, joins 8.5g polyvinyl alcohol in magnesium acetate solution.Then react by fluorine source with containing the magnesium source solution co-precipitation of polyvinyl alcohol, and open magnetic agitation simultaneously, react 2 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 80 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 350 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, roasting 2 hours removing charcoal templates in last retort furnace under 500 DEG C of air atmospheres, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 137m
2/ g.
Embodiment 9
Prepare the NH of the isopyknic 2mol/L of each 100ml
4the MgC of F solution and 1mol/L
2o
4.2H
2o solution, and in ammonium fluoride solution, add resol 6.1g.Mixed by anti-addition, and open magnetic agitation simultaneously, react 7 hours at the temperature of 30 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 100 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 400 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, finally 300 DEG C containing 10% oxygen and 90% nitrogen mixture atmosphere under tubular type kiln roasting 2 hours removing charcoal templates, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 233m
2/ g.
Embodiment 10
Prepare the NH of the isopyknic 2mol/L of each 100ml
4the MgCl of F solution and 1mol/L
2solution, and in ammonium fluoride solution, add resol 3.1g.Mixed by anti-addition, and open magnetic agitation simultaneously, react 3 hours at the temperature of 50 DEG C, then constant temperature leaves standstill aging 2 hours, by the pre-carbonization of baking oven 6 hours of putting into 100 DEG C after the solution evaporate to dryness of gained, then pre-carbonization 6 hours in the baking oven of 160 DEG C, in retort furnace under 400 DEG C of nitrogen atmospheres, namely roasting obtains the magnesium fluoride containing charcoal for 4 hours, last tubular type kiln roasting under 500 DEG C of air atmospheres 12 hours removing charcoal templates, can obtain the magnesium fluoride of high-ratio surface, its specific surface area is 93m
2/ g.
Above embodiment is only illustrative rather than definitive thereof technical scheme of the present invention, although with reference to above-described embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: still can modify to the present invention or equivalent replacement, and not departing from any amendment and the local replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (10)
1. the preparation method of a magnesium fluoride, comprise: make the magnesium source aqueous solution and fluorine source aqueous solution, also containing carbon source in gained mixed solution, described carbon source is sucrose, glucose, furfuryl alcohol, P123, polyvinyl alcohol, the mixture of one or more in resol, the mol ratio in carbon source and magnesium source counts 1 ~ 10:1 with C:Mg, the magnesium fluoride presoma that aging removing moisture obtains carbonaceous sources is left standstill after stirring lower fully reaction, again by the pre-carbonization in the temperature range of 80 ~ 160 DEG C in oxygen-containing atmosphere of the magnesium fluoride presoma of carbonaceous sources, then under the temperature condition of 350 ~ 400 DEG C, carbonization obtains the magnesium fluoride of doping charcoal in an inert atmosphere, finally by oxygen-containing atmosphere under the temperature condition of 300 ~ 500 DEG C high temperature removal charcoal obtain magnesium fluoride product.
2. the preparation method of magnesium fluoride as claimed in claim 1, it is characterized in that: magnesium source adopts the mixture of one or more in magnesium acetate, magnesium oxalate, magnesium nitrate, magnesium chloride, fluorine source adopts the mixture of one or more in Neutral ammonium fluoride, Potassium monofluoride, Sodium Fluoride.
3. the preparation method of magnesium fluoride as claimed in claim 1, is characterized in that: the mol ratio in carbon source and magnesium source counts 3 ~ 6:1 with C:Mg.
4. the preparation method of magnesium fluoride as claimed in claim 3, is characterized in that: the mol ratio in carbon source and magnesium source counts 4:1 with C:Mg.
5. the preparation method of the magnesium fluoride as described in one of Claims 1 to 4, is characterized in that: the reaction in fluorine source and magnesium source is carried out under the temperature condition of 20 ~ 80 DEG C, and the reaction times is 0.5 ~ 10 hour.
6. the preparation method of the magnesium fluoride as described in one of Claims 1 to 4, is characterized in that: described oxygen-containing atmosphere is air atmosphere or oxygen-containing gas volume concentrations is the nitrogen atmosphere of 1 ~ 50%.
7. the preparation method of the magnesium fluoride as described in one of Claims 1 to 4, is characterized in that: pre-carbonization time is 5 ~ 20 hours;
Carbonization time is 1 ~ 10 hour;
Reaction times is 2 ~ 12 hours.
8. the preparation method of magnesium fluoride as claimed in claim 7, is characterized in that: carbonization time is 2 ~ 5 hours.
9. the preparation method of magnesium fluoride as claimed in claim 7, it is characterized in that: described high temperature removal charcoal carries out under the temperature condition of 350 ~ 500 DEG C, the reaction times is 4 ~ 6 hours.
10. the preparation method of the magnesium fluoride as described in claim 3 or 4, is characterized in that the preparation method of described magnesium fluoride carries out in accordance with the following steps:
(1) make the magnesium source aqueous solution and fluorine source aqueous solution, also containing carbon source in gained mixed solution, the mol ratio in carbon source and magnesium source counts 1 ~ 10:1 with C:Mg, in 20 ~ 80 DEG C of reactions 2 ~ 10 hours under stirring, stops stirring; Described carbon source adopts the mixture of one or more in sucrose, glucose, furfuryl alcohol, P123, polyvinyl alcohol, resol; Described magnesium source adopts the mixture of one or more in magnesium acetate, magnesium oxalate, magnesium nitrate, magnesium chloride; Described fluorine source adopts the mixture of one or more in Neutral ammonium fluoride, Potassium monofluoride, Sodium Fluoride;
(2) the reaction solution constant temperature that step (1) obtains is left standstill aging removing moisture, obtain the magnesium fluoride presoma of carbonaceous sources;
(3) the magnesium fluoride presoma of carbonaceous sources is first under an oxygen-containing atmosphere in 80 ~ 160 DEG C of charings 5 ~ 20 hours in advance, then carbonization 2-5 hour at 350 ~ 400 DEG C of temperature under an inert atmosphere, the magnesium fluoride of the charcoal that obtains adulterating;
(5) magnesium fluoride of doping charcoal is under an oxygen-containing atmosphere in 300 ~ 500 DEG C of roastings carbon removal in 2 ~ 12 hours, obtains magnesium fluoride product.
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