CN1803611A - Method for preparing nanometer borofluoride powder - Google Patents
Method for preparing nanometer borofluoride powder Download PDFInfo
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- CN1803611A CN1803611A CN 200610001866 CN200610001866A CN1803611A CN 1803611 A CN1803611 A CN 1803611A CN 200610001866 CN200610001866 CN 200610001866 CN 200610001866 A CN200610001866 A CN 200610001866A CN 1803611 A CN1803611 A CN 1803611A
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- borofluoride
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Abstract
The invention relates to a preparation method for nano M(BF4)n powder, which comprises: dissolving excess dried BF3 into organic solvent to mix with dried anhydrous MFn powder by the ratio 1:1.1-1:2.5; putting into sealed stainless steel tank with diameter as mm phi5:phi1:phi0.2=1:3:5 for high-energy grinding 50-70h as the chemical reaction equation MFn+nBF3->M(BF4)n; then, removing the steel by magnetic field, absorbing and volatilizing excess BF3 solution and solvent, and obtaining the product with size 50-80nm. This invention is simple and convenient to control, and has low cost and no pollution.
Description
Technical field
The invention belongs to field of powder metallurgy preparation, particularly a kind of nanometer borofluoride M (BF
4)
nThe preparation method of powder.
Background technology
In the prior art, nanometer powder is meant the ultra-fine grain of median size below 100nm.Reasons such as the atom number atom few, surface arrangement in, the particle little owing to its volume is many, its surface-area effects, volume effect and small-size effect make it have the performance that is different from conventional bulk and micropowder material, all show unusual characteristic at aspects such as light, electricity, magnetic, heat and chemistry, Aeronautics and Astronautics, military project, material, metallurgy, chemical industry, medicine and other fields have many new, very important use is worth, and is described as brand-new new function material.This just new function material of nanometer borofluoride powder with brand-new function.Conventional fluoroborate is important metallurgy of a class and chemical industry raw material, it can be used as resination catalyzer, oxidation retarder, fire retardant, gas fusing assistant, be used for refining fluxing agent, grain-refining agent, coating, the fluorizating agent of non-ferrous metal and be used as chemical reagent etc., also can be used as the surface treatment that solvent is used for light metal processing.And nanometer borofluoride powder, compare with conventional borofluoride powder, because activity is bigger, not only keep and improved outside the above-mentioned performance, up-to-date research also shows, nanometer borofluoride powder still is fabulous extreme pressure antiwear agent for lubricant oil, and the lubricating oil that contains fluoroborate has superpower lubricated, antifriction and wear-resistant function.This is found, has not only widened the Application Areas of fluoroborate, has injected new life also for the research of friction and lubrication technology.
What at present, industrial preparation fluoroborate was the most frequently used is aqueous acid medium alkali neutralisation:
Or
But because fluoroborate is slightly soluble in water or soluble in water, the particle diameter of the fluoroborate that very easily crystal growth, so general chemical process makes is 10-50 μ m, is difficult to prepare the nano level borofluoride powder.
High-energy ball milling method is another method of preparation nanometer particle, and it is rotation or the vibration that utilizes ball mill, makes hard grind ball wherein carry out the intensive bump, grind and stir raw material, powder is pulverized be the method for nano_scale particle.High-energy ball milling method be applicable to processing hard relatively, fragile materials.Have advantages such as output height, technology are simple because high-energy ball milling method prepares nanometer powder, become a kind of important method of preparation nanometer powder in recent years.To prepare nanometer powder be a very difficult job but adopt high-energy ball milling method directly to grind fluoroborate, also can only obtain particle about 300nm through long grinding, and grind for a long time, and the abrading-ball badly broken causes abrasive material to pollute.
Summary of the invention
The object of the present invention is to provide a kind of technology, equipment is simple, easy to control, cost is low, the preparation method of the free of contamination nano level borofluoride powder of abrasive material.
According to above-mentioned purpose, technical scheme of the present invention is: utilize BF
3Can be dissolved in the characteristic of some organic solvent (for example kerosene), adopt high-energy ball milling technology, under the situation that does not have water to participate in, fully react and made nano level borofluoride powder with anhydrous fluoride salt powder, this method has been avoided the crystal growth of fluoroborate in water, prepare the nano level fluoroborate particle that prior art can't make, particle diameter reaches 50-80nm.
According to above-mentioned purpose and technical scheme, technology of the present invention comprises step specific as follows:
1, at first with excessive dry BF
3Be dissolved in the organic solvent;
2, get the anhydrous fluoride salt MF of exsiccant then
nPowder and above-mentioned BF
3Solution mixes by a certain percentage, MF
nPowder and BF
3Mol ratio be 1: 1.1-1: 2.5, pack into the sealing stainless steel jar mill in, be equipped with stainless steel ball radius mm φ 5: φ 1: φ 0.2=1: 3: 5, carry out high-energy ball milling 50-70h, above-mentioned chemical equation is:
；
3, after above-mentioned reaction is finished, utilize the effect in magnetic field to remove Stainless Steel Ball, suction strainer also vapors away excessive BF
3And organic solvent, just obtaining nano level borofluoride powder, the particle diameter of powder can reach 50-80nm.
Organic solvent is a kerosene in the technique scheme, anhydrous fluoride salt MF
nPowder is CaF
2, MgF
2, KF, NaF, NH
4Among the F any.
The principle of work of above-mentioned concrete technical scheme is:
1, key point of the present invention is to adopt anhydrous fluoride salt MF
nIn the presence of certain medium with BF
3In high energy ball mill, can take place to grind chemical combination, prepare nano level fluoroborate M (BF
4)
nPowder can not have water to participate in the reaction process, avoid the product crystal growth.
2, with excessive exsiccant BF
3Be dissolved in the organic solvent.BF
3Normal temperature is down colourless gas, has pungent odour, is soluble in the vitriol oil, concentrated nitric acid, kerosene, benzene, tetracol phenixin or oil of mirbane etc., and is water-soluble and resolve into boric acid and fluoroboric acid, and emit heat.Consider toxicity problem, the present invention is with BF
3Be dissolved in the kerosene.
3, get the anhydrous fluoride salt MF of exsiccant
nPowder and above-mentioned BF
3Kerosin mixes by a certain percentage, in the stainless steel jar mill of the sealing of packing into, is equipped with the stainless steel abrading-ball, carries out high-energy ball milling.In mechanical milling process, the fluoride salt particle fragmentation produces the high energy interface, has quickened fluoride salt and BF
3Combination reaction, this combination reaction produces new lattice imperfection in that particle is inner again, has quickened the fragmentation of particle, these two kinds of effects are mutually promoted, and strengthen mutually, have finally made nano level fluoroborate.
The present invention compared with prior art has preparation technology, equipment is simple, easy to control, cost is low, the free of contamination advantage of abrasive material.Above-mentioned advantage is specially: this patent prepares nano level fluoroborate M (BF
4)
nMethod, utilized BF
3Can be dissolved in the characteristic of some organic solvent (for example kerosene), adopt the method for high-energy ball milling reaction, in the presence that does not have water, made nano level borofluoride powder, avoided the crystal growth of fluoroborate in water, made the nano level fluoroborate particle that prior art can't make, and experimental installation has been simple, only need a high energy ball mill, raw material is easy to get, and cost is low, and the nano particle diameter that makes is 50-80nm.
Embodiment
Adopt preparation method of the present invention, prepared 5 batches of nanometer borofluoride powders, table 1 is the raw materials used and preparation technology parameter table of the embodiment of the invention, with the median size of having advanced to list the nanometer borofluoride powder that makes.Wherein 1-5# is the embodiment of the invention.
Table 1 the present invention prepares the raw materials used and preparation technology parameter table of nano level borofluoride powder
| Sample number | Reactant | Resultant | Preparation technology parameter | |||
| MF nSalt | BF 3 | Its ratio mol/mol | M(BF 4) n | Particle diameter nm | Ball milling time h | |
| 1 | CaF 2 | 1∶2.4 | Ca(BF 4) 2 | 73 | 50 | |
| 2 | MgF 2 | 1∶2.2 | Mg(BF 4) 2 | 67 | 60 | |
| 3 | KF | 1∶1.8 | KBF 4 | 53 | 70 | |
| 4 | NaF | 1∶1.5 | NaBF 4 | 62 | 60 | |
| 5 | NH 4F | 1∶1.2 | NH 4BF 4 | 79 | 50 | |
Claims (3)
1, a kind of preparation method of nanometer borofluoride powder is characterized in that this method comprises following concrete steps:
A, at first with excessive exsiccant BF
3Be dissolved in the organic solvent;
B, get the anhydrous fluoride salt MF of exsiccant then
nPowder and above-mentioned BF
3Solution mixes by a certain percentage, MF
nPowder and BF
3Mol ratio be 1: 1.1-1: 2.5, pack into the sealing stainless steel jar mill in, be equipped with stainless steel ball radius mm φ 5: φ 1: φ 0.2=1: 3: 5, carry out high-energy ball milling 50-70h, above-mentioned chemical equation is:
After c, above-mentioned reaction are finished, utilize the effect in magnetic field to remove Stainless Steel Ball, suction strainer also vapors away excessive BF
3And organic solvent, just obtaining nano level borofluoride powder, the particle diameter of powder can reach 50-80nm.
2, the preparation method of nanometer borofluoride powder according to claim 1 is characterized in that organic solvent is a kerosene.
3, the preparation method of nanometer borofluoride powder according to claim 1 is characterized in that anhydrous fluoride salt MF
nPowder is CaF
2.MgF
2.KF, NaF, NH
4Among the F any.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610001866 CN1803611A (en) | 2006-01-25 | 2006-01-25 | Method for preparing nanometer borofluoride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610001866 CN1803611A (en) | 2006-01-25 | 2006-01-25 | Method for preparing nanometer borofluoride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1803611A true CN1803611A (en) | 2006-07-19 |
Family
ID=36865790
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610001866 Pending CN1803611A (en) | 2006-01-25 | 2006-01-25 | Method for preparing nanometer borofluoride powder |
Country Status (1)
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|---|---|
| CN (1) | CN1803611A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289195B (en) * | 2007-04-19 | 2010-08-04 | 多氟多化工股份有限公司 | Process for preparing potassium borofluoride and co-production of white carbon black and sodium fluosilicate |
| CN105776237A (en) * | 2016-03-30 | 2016-07-20 | 云南铁坦新材料科技股份有限公司 | Synthesis method of calcium fluoborate hydrate |
-
2006
- 2006-01-25 CN CN 200610001866 patent/CN1803611A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289195B (en) * | 2007-04-19 | 2010-08-04 | 多氟多化工股份有限公司 | Process for preparing potassium borofluoride and co-production of white carbon black and sodium fluosilicate |
| CN105776237A (en) * | 2016-03-30 | 2016-07-20 | 云南铁坦新材料科技股份有限公司 | Synthesis method of calcium fluoborate hydrate |
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|---|---|---|---|
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| ASS | Succession or assignment of patent right |
Owner name: GAUNA BEIJING INSTITUTE OF TECHNOLOGY CO. Free format text: FORMER OWNER: IRON AND STEEL RESEARCH GEUERAL INST. Effective date: 20080523 |
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Effective date of registration: 20080523 Address after: Beijing City, Haidian District Daliushu Village No. 19 post encoding: 100081 Applicant after: BEIJING CISRI-GAONA MATERILALS & TECHNOLOGY Co., LTD. Address before: 76, College Road South, Beijing, Haidian District: 100081 Applicant before: Central Iron & Steel Research Institute |
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Open date: 20060719 |