CN105347366A - Preparing method of nanoscale magnesium oxide micropowder - Google Patents
Preparing method of nanoscale magnesium oxide micropowder Download PDFInfo
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- CN105347366A CN105347366A CN201510937347.3A CN201510937347A CN105347366A CN 105347366 A CN105347366 A CN 105347366A CN 201510937347 A CN201510937347 A CN 201510937347A CN 105347366 A CN105347366 A CN 105347366A
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- micro mist
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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- 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
- C01P2006/12—Surface area
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- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparing method of nanoscale magnesium oxide micropowder. The preparing method comprises following steps in sequence: adopting a method combining a direct sediment method and a microwave water bath heating method, taking crystal magnesium sulfate and anhydrous sodium carbonate as raw materials, dissolving by taking water as a solvent, then adding a surfactant into the solution, stirring uniformly, placing mixed liquid into a microwave oven for water bath heating, washing with distilled water and dispersing an obtained precursor, then placing in the oven for drying, and finally placing the dried precursor into a muffle furnace for roasting to obtain the nanoscale magnesium oxide micropowder. The obtained nanoscale magnesium oxide micropowder product is simple in procedure, low in cost, good in performance, higher in purity, controllable in particle size and suitable for industrialized production.
Description
Technical field
The present invention relates to magnesian preparation method, particularly a kind of preparation method of nanoscale magnesium micro mist.
Background technology
Magnesium oxide is had many uses, can be used as refractory materials, pot, refractory brick etc. is increased as material of construction for the manufacture of pottery, magnesia carbon brick, magnesium, it and magnesium chloride or Adlerika are mixed and made into magnesia cement or light-duty heat-insulating shield etc. in metallurgical industry, obtain MAGNESIUM METAL with ferrosilicon or carbon reduction-oxidation magnesium 2000 DEG C time.In addition, in Steel industry, rubber industry, medicine, paint, papermaking, agricultural, makeup etc., important purposes is had.
Nano magnesia is a kind of novel high function fine inorganic material, due to the singularity of its structure, determines it and has the electricity, magnetics, calorifics and the optical property that are different from body.Along with the granular of particle, the specific surface area of nano magnesia enlarges markedly, and surface energy raises, and shows high surface, strong adsorptivity and good low-temperature sintering.
Adopt and make catalyzer through certain pretreated nano magnesia, the yield catalyzing and synthesizing legal system second phthalein acetone process product can be made to bring up to 95% by 85%.Nano magnesia also has very high catalytic activity to the polymerization of Malaysia phthalimide.
Nano magnesia can be effective as the agglutinant stablizer of other potteries such as silicon oxide, aluminum oxide, ferric oxide, and can be processed into sintered compact, has very important purposes at electronic material and ceramic field.Nano magnesia has good sterilizing function.The bactericidal property of u s company to nano magnesia has done systematic research, result shows that the magnesium oxide of 4 ~ 10nm has abnormal outstanding killing effect (in 20min, the killing effect of bacterium is 100%) to multiple virus, bacterium and fungi, and the killing effect being much better than bacterium in common silver system sterilant is.Nano magnesia has huge adsorptive power to gas, the gas of adsorbable own wt 20%.
The preparation of current nanoscale magnesium powder mainly contains two kinds of modes, and one is Physical, i.e. the mode of Mechanical Crushing, and two is chemical methods, comprises vapor phase process, liquid phase method etc.On overall, there are following various problems in above introduced preparing in the technique of nano magnesia and nano-powder: the control of the reunion of primary particle and bad dispersibility, powder surface anomalad roughness and surface properties is difficult, the control difficulty of technology stability greatly, the problems such as the poor stability of powder, environmental pollution be large.
Summary of the invention
In order to overcome Problems existing in existing nanoscale magnesium technique, the invention provides a kind of preparation method of nanoscale magnesium micro mist.
The object of the invention is to be reached by following measures: the preparation method that a kind of nanoscale magnesium micro mist is provided, in turn include the following steps: with crystalline sulfuric acid magnesium and anhydrous sodium carbonate for raw material, be after dissolution with solvents with water, tensio-active agent is added in solution, stir, mixed solution is put into microwave oven heating in water bath, after the precursor distilled water wash obtained, dispersion, put into baking oven to dry, finally the precursor after oven dry is put into retort furnace roasting, namely obtain nano magnesia micro mist.
Further, the precipitation agent used in described process is anhydrous Na CO
3, itself and raw material MgSO
47H
2the mol ratio of O is 1 ~ 2:1, and preferred version is material molar ratio is 1:1.
Further, the tensio-active agent added in described process be polyoxyethylene glycol, polyvinyl butyral, Sodium dodecylbenzene sulfonate a kind of mixture of or arbitrary combination, its add-on is 10% ~ 15% of liquor capacity, preferred version is for selecting cetomacrogol 1000 as tensio-active agent, and its add-on is 15% of liquor capacity.
Further, the processing condition of described microwave water-bath are microwave power is 550 ~ 600W, and microwave water-bath heat-up time is 30 ~ 50min.
Further, in described distilled water wash process, washing times is 3 ~ 5 times, and preferred version is distilled water wash three times.
Further, in described roasting process, processing condition are optimum calcination temperature is 500 ~ 600 DEG C, and roasting time is 1.5 ~ 2h, and preferred version is calcine 1.5h at 500 DEG C.
Beneficial effect: the present invention utilizes direct precipitation method to combine with microwave water bath heating to prepare nanometer magnesia powder has the advantages that speed of response is fast, reaction conditions is gentle, reaction efficiency is high, and obtained product production is high, steady quality, and easy control of reaction conditions, cheap, operation is simple, has splendid industrial prospect.
Embodiment
Below by embodiment, the present invention is described in detail.
The invention provides a kind of preparation method of nanoscale magnesium micro mist, in turn include the following steps: with crystalline sulfuric acid magnesium and anhydrous sodium carbonate for raw material, be after dissolution with solvents with water, in solution, add tensio-active agent, stir, mixed solution is put into microwave oven heating in water bath, after the precursor distilled water wash obtained, dispersion, put into baking oven to dry, finally the precursor after oven dry is put into retort furnace roasting, namely obtain nano magnesia micro mist.
Further, the precipitation agent used in described process is anhydrous Na CO
3, itself and raw material MgSO
47H
2the mol ratio of O is 1 ~ 2:1, and preferred version is material molar ratio is 1:1.
Further, the tensio-active agent added in described process be polyoxyethylene glycol, polyvinyl butyral, Sodium dodecylbenzene sulfonate a kind of mixture of or arbitrary combination, its add-on is 10% ~ 15% of liquor capacity, preferred version is for selecting cetomacrogol 1000 as tensio-active agent, and its add-on is 15% of liquor capacity.
Further, the processing condition of described microwave water-bath are microwave power is 550 ~ 600W, and microwave water-bath heat-up time is 30 ~ 50min.
Further, in described distilled water wash process, washing times is 3 ~ 5 times, and preferred version is distilled water wash three times.
Further, in described roasting process, processing condition are optimum calcination temperature is 500 ~ 600 DEG C, and roasting time is 1.5 ~ 2h, and preferred version is calcine 1.5h at 500 DEG C.
Embodiment
Take the MgSO of 125g respectively
47H
2the anhydrous sodium carbonate of O and 53g, add in the water of 1L, then the dispersion agent cetomacrogol 1000 of 150ml is added wherein, after stirring, mixed solution is placed in the water-bath (200ml) that microwave power is 550W and heats 30min, the magnesiumcarbonate precipitation obtained, with distilled water wash 3 times, put into baking oven, drying is carried out at the temperature of 120 DEG C, finally by dry precursor put into retort furnace, at 500 DEG C of temperature, calcining 1.5h, namely nanoscale magnesium micro mist 113.6g is obtained, after measured, the specific surface area obtaining nanometer magnesia powder is 183.35m2/g.
Above content is the further description done the present invention in conjunction with optimal technical scheme, can not assert that the concrete enforcement of invention is only limitted to these explanations.Concerning general technical staff of the technical field of the invention, under the prerequisite not departing from design of the present invention, simple deduction and replacement can also be made, all should be considered as protection scope of the present invention.
Claims (6)
1. the preparation method of a nanometric magnesium hydroxide micro mist, it is characterized in that, in turn include the following steps: with crystalline sulfuric acid magnesium and anhydrous sodium carbonate for raw material, be, after dissolution with solvents, in solution, add tensio-active agent with water, stir, mixed solution is put into microwave oven heating in water bath, after the precursor distilled water wash obtained, dispersion, put into baking oven and dry, finally the precursor after oven dry is put into retort furnace roasting, namely obtain nano magnesia micro mist.
2. the preparation method of a kind of nanoscale magnesium micro mist according to claim 1, it is characterized in that, the precipitation agent used in described process is anhydrous Na CO
3, itself and raw material MgSO
47H
2the mol ratio of O is 1 ~ 2:1.
3. the preparation method of a kind of nanoscale magnesium micro mist according to claim 1, is characterized in that, the processing condition of described microwave water-bath are microwave power is 550 ~ 600W, and microwave water-bath heat-up time is 30 ~ 50min.
4. the preparation method of a kind of nanoscale magnesium micro mist according to claim 1, is characterized in that, in described distilled water wash process, washing times is 3 ~ 5 times.
5. the preparation method of a kind of nanoscale magnesium micro mist according to claim 1, is characterized in that, in described roasting process, processing condition are optimum calcination temperature is 500 ~ 600 DEG C, and roasting time is 1.5 ~ 2h.
6. the preparation method of a kind of nanoscale magnesium micro mist according to claim 1, it is characterized in that, the tensio-active agent added in described process be polyoxyethylene glycol, polyvinyl butyral, Sodium dodecylbenzene sulfonate a kind of mixture of or arbitrary combination, its add-on is 10% ~ 15% of liquor capacity.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105858691A (en) * | 2016-05-18 | 2016-08-17 | 四川大学 | Method for preparing flower-like magnesium oxide microsphere according to precipitation method |
CN111909803A (en) * | 2020-09-17 | 2020-11-10 | 广州市白云区大荣精细化工有限公司 | Clothes fragrance-retaining composition and preparation method thereof |
CN114106587A (en) * | 2021-12-13 | 2022-03-01 | 辽宁科技大学 | Method for preparing electrical-grade coated magnesium oxide by using environment-friendly ester solvent |
CN114940503A (en) * | 2022-04-29 | 2022-08-26 | 宝鸡文理学院 | Method for preparing nano magnesium oxide in ionic liquid by microwave heating and application thereof |
-
2015
- 2015-12-15 CN CN201510937347.3A patent/CN105347366A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105858691A (en) * | 2016-05-18 | 2016-08-17 | 四川大学 | Method for preparing flower-like magnesium oxide microsphere according to precipitation method |
CN111909803A (en) * | 2020-09-17 | 2020-11-10 | 广州市白云区大荣精细化工有限公司 | Clothes fragrance-retaining composition and preparation method thereof |
CN114106587A (en) * | 2021-12-13 | 2022-03-01 | 辽宁科技大学 | Method for preparing electrical-grade coated magnesium oxide by using environment-friendly ester solvent |
CN114940503A (en) * | 2022-04-29 | 2022-08-26 | 宝鸡文理学院 | Method for preparing nano magnesium oxide in ionic liquid by microwave heating and application thereof |
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