CN101353176A - Novel method for preparing nano-magnesia - Google Patents
Novel method for preparing nano-magnesia Download PDFInfo
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- CN101353176A CN101353176A CNA2007101375211A CN200710137521A CN101353176A CN 101353176 A CN101353176 A CN 101353176A CN A2007101375211 A CNA2007101375211 A CN A2007101375211A CN 200710137521 A CN200710137521 A CN 200710137521A CN 101353176 A CN101353176 A CN 101353176A
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Abstract
The invention relates to the preparation technology of nano materials, in particular to a new method for preparing nano-magnesia powder, which belongs to the technical field of inorganic chemical industry and nano materials. In the invention, magnesia is taken as raw material and directly converted into a precursor of the nano-magnesia by ammonium carbonate or ammonium bicarbonate, an activator is taken as a microemulsion reactor for conversion reaction, that is, the conversion reaction is carried out under the protection of an organic solvent. Ammonia generated by the conversion reaction is absorbed by water and reacts with carbon dioxide collected by calcined basic magnesium carbonate to generate the ammonium carbonate (or the ammonium hydrogen carbonate) which is taken as raw material for spare use, simultaneously the precipitated mother liquor of the precursor is a mixture of the ammonium carbonate and the ammonium hydrogen carbonate and can be recycled. The prepared precursor is dried in vacuum, and calcined at a high temperature to obtain the nano-magnesia. The prepared nano-magnesia has low agglomeration degree, uniform particle distribution, tiny average particle size (not greater than 30nm), large specific surface area (not less than 150m<2>/g), cheap and readily available raw materials, simple technology and short process flow and convenient operation, thus being beneficial to realizing industrialized production.
Description
Technical field
The present invention relates to the technology of preparing of nano material, particularly prepare the novel method of nano magnesia powder, belong to inorganic chemical industry and technical field of nano material.
The technical background nano magnesia is a kind of new function fine inorganic material that is born along with the development of nano material technology, its particle diameter is between 1～100nm, be widely used in fields such as advanced ceramic, electrical apparatus insulation, fire-retardant, makeup, face powder, paint, rubber filler, sour gas sorbent material, support of the catalyst, wide application prospect and huge economic potential are arranged.
Nano magnesia synthetic has vapor phase process, solid phase method, liquid-phase precipitation method.Vapor phase process is big to equipment and technical requirements height and energy consumption, contaminate environment; The solid phase rule is difficult to prepare particle diameter less than the product of 100nm and to the equipment requirements height; Liquid-phase precipitation method is simple to operate, and raw material is easy to get, and productive rate is big, is a kind of industrialized synthetic method that is easy to.But liquid-phase precipitation method is to add precipitation agent in containing one or more ionic soluble salt solution, generating precipitation under certain condition separates out from mother liquor, removal of impurities difficulty technically, have in technical process that Production Flow Chart is long, energy consumption is high, big and the skewness of product granularity is arranged on quality product, be difficult to control shortcomings such as shape in the preparation.
Chinese patent CN 1539774A, with the magnesite light burnt powder is raw material, adopt the means that stir the mill reinforcing mass transfer, realize the light calcined magnesia carbonization down at 10～40 ℃, carbonization time is 1～5 hour, the carbodiimide solution filtration is obtained magnesium bicarbonate solution, 80～100 ℃ of pyrolysis, form precipitation, after filtration, dry, calcining makes nano magnesia, its median size is 15～50nm, and product purity is 98.7%.
Chinese patent CN 1597520A, with urea and magnesium salts is to be mixed with the aqueous solution that magnesium ion concentration is 1～4mol/L in 2: 1～6: 1 in molar ratio, add-on is the dispersion agent of magnesium salts quality 1～5% simultaneously, heating in water bath to 348～373K, ageing behind reaction 2～6h, suction filtration, with absolute ethanol washing and with after the supercritical co drying, calcining makes the nano magnesia powder under 623～923K.This method has solved the generation of precipitin reaction and drying process particle cluster aggressiveness well, and the product monodispersity is good, and specific surface area is big, and the presoma of its product is a magnesium hydroxide.
The present invention be exactly propose for shortcoming such as solve liquid-phase precipitation method technical process complexity, energy consumption height, grain diameter is big, size-grade distribution is inhomogeneous, shape is difficult to control a kind of brand-new, greatly shortened process, reduce the particle aggregation chance, precipitation transforms and one step of emulsification finishes new production technique.
Summary of the invention
This technology is raw material with light calcined magnesia and industrial volatile salt (or bicarbonate of ammonia); under the effect of promoting agent; magnesium oxide and volatile salt (or bicarbonate of ammonia) direct reaction; conversion reaction is the micro emulsion reactor with the promoting agent; promptly under the organic solvent protection, carry out conversion reaction, prepare the presoma of nano magnesia.Again with its vacuum constant temperature drying, and calcining at high temperature, make nano magnesia.Its concrete steps are described below:
(1), light calcined magnesia is levigate, its granularity is reached below the 0.075mm, cofabrication good concentration is 0.05～2.0mol/L volatile salt (or bicarbonate of ammonia) solution for standby.
(2), will be that 0.5: 1～2: 1 volatile salt (or bicarbonate of ammonia) solution adds in the reactor with the magnesium oxide mol ratio, drip promoting agent, its amount is 0.1 ‰～10 ‰ of solution total mass, behind ultra-sonic dispersion 1～10min, adding light-magnesite powder under certain stir speed (S.S.) reacts, be warming up to 50～100 ℃ rapidly, its temperature rise rate is controlled at 5～10 ℃/min.
(3), reach 50～100 ℃ when temperature of reaction system, under this temperature, continue reaction 0.5～2h, obtain the basic carbonate magnesium latex emulsion.Simultaneously, the ammonia water that steams is absorbed, the carbon dioxide reaction of collecting with the calcining magnesium basic carbonate generates volatile salt (or bicarbonate of ammonia) as raw material for standby.
(4), with the basic carbonate magnesium latex emulsion vacuum filtration of gained, filtrate mainly is volatile salt and ammonium bicarbonate soln, can be used as the raw material recycle; Behind the filter cake usefulness deionized water wash 2～3 times, use absolute ethanol washing again 1～2 time,, obtain the nano magnesia presoma in 60～100 ℃ of vacuum-dryings (vacuum tightness is 0.02Pa), 1～4h.
(5), the presoma that makes is calcined 1～3h down at 500～800 ℃ and make nano oxidized magnesium products.
Wherein, described magnesium oxide is magnesite calcining gained (or light magnesium oxide), its quality percentage composition 〉=95%.
Described promoting agent is: polyalcohols promoting agent, for example PEG, PEG400, PEG600 etc.; Or organic ammonium salt promoting agent, for example methylformamide, methylacetamide etc.; Or fatty alcohol ether sulphate; Or its compound, its mass ratio is (0.1～2.1): 1: (0～1.5).
Described volatile salt (or bicarbonate of ammonia) strength of solution is 0.05～2mol/L;
Described stir speed (S.S.) is 1000～5000r/min, adjusts rotating speed according to the desired product particle diameter.
Compared with prior art, the present invention has following advantage:
The nano magnesia reunion degree that A makes is little, and size distribution is even, and median size is 20nm～50nm, the big and steady quality of specific surface area;
B adopts direct conversion method, and technology is simple and flow process short, is easy to realize suitability for industrialized production;
C reaction conditions gentleness, to equipment require low, productive rate 〉=95%;
D preparation process material is realized closed cycle, and no waste liquid waste gas produces, and belongs to green preparation process.
E the inventive method both can be produced nano magnesia, but the magnesium basic carbonate of production nanometer again.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
It below is exemplifying embodiment of the present invention.
Embodiment 1
(1), in the ammonium carbonate solution of 150ml 0.8mol/l, adds the 0.03g methylacetamide, transfer to the there-necked flask of 250ml behind the ultra-sonic dispersion 3min, add 1.5g magnesium oxide simultaneously, start stirrer (speed is 1200r/min), heating in water bath to 60 ℃, reaction 1.5h, naturally cool to room temperature, vacuum filtration is used deionized water wash 3 times, use absolute ethanol washing again 3 times, to guarantee that water is replaced fully.
(2), product that (1) is obtained puts into vacuum drying oven (vacuum tightness is 0.02Pa), at 80 ℃ of following vacuum-drying 2h.
(3), dried sample is at 600 ℃ of following calcining 2h, obtains the magnesium oxide powder that median size is 30nm.
Embodiment 2
(1), in the ammonium carbonate solution of 150ml 0.8mol/l, adds the 0.04g fatty alcohol ether sulphate, transfer to the there-necked flask of 250ml behind the ultra-sonic dispersion 3min, add 1.3g magnesium oxide simultaneously, start stirrer (speed is 1200r/min), heating in water bath to 60 ℃, reaction 1.5h, naturally cool to room temperature, vacuum filtration is used deionized water wash 3 times, use absolute ethanol washing again 3 times, to guarantee that water is replaced fully.
(2), product that (1) is obtained puts into vacuum drying oven (vacuum tightness is 0.02Pa), at 80 ℃ of following vacuum-drying 2h.
(3), dried sample is at 550 ℃ of following calcining 2h, measures through transmission electron microscope and specific surface area, obtaining the magnesium oxide powder median size is 26nm, specific surface area is 164.44m
2/ g.
Embodiment 3
(1), in the ammonium bicarbonate aqueous solution of 150ml 1.5mol/l, adds 0.20g PEG400, transfer to the there-necked flask of 250ml behind the ultra-sonic dispersion 3min, add 1.8g magnesium oxide simultaneously, start stirrer (rotor speed is 1200r/min), heating in water bath to 90 ℃, reaction 1.5h, naturally cool to room temperature, vacuum filtration is used deionized water wash 3 times, use absolute ethanol washing again 3 times, to guarantee that water is replaced fully.
(2), product that (1) is obtained puts into vacuum drying oven (vacuum tightness is 0.02Pa), at 80 ℃ of following vacuum-drying 2h.
(3), dried sample is at 600 ℃ of following calcining 2h, measures through transmission electron microscope, the magnesium oxide powder median size that obtains is 20nm.
Claims (9)
1, a kind of direct conversion method prepares the processing method of nano magnesia, it is characterized in that, with magnesium oxide and volatile salt (bicarbonate of ammonia) is raw material, under the promoting agent effect, magnesium oxide and volatile salt (bicarbonate of ammonia) reaction is converted into the presoma of nano magnesia, through vacuum-drying, high-temperature calcination, make nano magnesia.
2, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that, the precipitation transforming agent is volatile salt (bicarbonate of ammonia) during conversion reaction.
3, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that, the mol ratio of magnesium oxide and volatile salt (bicarbonate of ammonia) is 1: 0.5～1: 2.
4, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that, described promoting agent is: polyalcohols promoting agent, for example PEG, PEG400, PEG600 etc.; Or organic amine salt promoting agent, for example methylformamide, methylacetamide etc.; Or fatty alcohol ether sulphate; Or the compound of three class promoting agents, its mass ratio is (0.1～2.1): 1: (0～1.5).Used active dose is 0.1 ‰～10 ‰ of a reaction system solution total mass.
5, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that, the concentration of volatile salt (bicarbonate of ammonia) solution should be 0.05～2mol/L, and the conversion reaction temperature is 50～100 ℃.
6, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that, the ammonia water of emitting during conversion reaction absorbs, and the carbon dioxide reaction of collecting with the calcining magnesium basic carbonate generates volatile salt (or bicarbonate of ammonia) as raw material for standby.
7, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that the presoma mother liquor is the mixture of volatile salt and bicarbonate of ammonia, can be used as the raw material recycle.
8, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that the presoma drying means is vacuum-drying (vacuum tightness is 0.02Pa), and drying temperature is 60～100 ℃, and be 1～4h time of drying.
9, direct conversion method according to claim 1 prepares the processing method of nano magnesia, it is characterized in that the presoma calcining temperature is 500～800 ℃, and calcination time is 1～3h, and its temperature rise rate is 15～100 ℃/min.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948299A (en) * | 2010-09-14 | 2011-01-19 | 西南科技大学 | Preparation method of compact magnesia ceramics by sintering |
| CN104495881A (en) * | 2014-12-19 | 2015-04-08 | 中南大学 | Process for preparing high-purity silicon steel magnesium oxide from magnesium hydroxide |
| CN105050955A (en) * | 2013-03-25 | 2015-11-11 | 神岛化学工业株式会社 | Magnesium oxide particles, resin composition, rubber composition, and molded article |
| CN105271318A (en) * | 2015-11-23 | 2016-01-27 | 中国科学院青海盐湖研究所 | Preparation method of magnesium oxide nanocrystalline |
| CN105271319A (en) * | 2015-10-28 | 2016-01-27 | 内江师范学院 | Method for preparing nanometer MgO |
| CN105776255A (en) * | 2014-11-25 | 2016-07-20 | 重庆文理学院 | Preparation method of spherical magnesium oxide particles with large specific surface area |
| CN108569712A (en) * | 2018-04-04 | 2018-09-25 | 内江师范学院 | Preparation method of tetragonal body shape magnesium oxide material and products thereof and application |
| CN111848161A (en) * | 2020-08-05 | 2020-10-30 | 上海大学(浙江·嘉兴)新兴产业研究院 | Preparation method of nano zirconia powder |
| CN113184883A (en) * | 2021-05-11 | 2021-07-30 | 青海施丹弗化工有限责任公司 | Method for continuously producing nano magnesium oxide |
| CN114408950A (en) * | 2022-02-22 | 2022-04-29 | 上海太洋科技有限公司 | Supported high-dispersion nano magnesium oxide and preparation method and application thereof |
| CN115784275A (en) * | 2022-11-29 | 2023-03-14 | 中南大学 | Green method for preparing high-purity light magnesium oxide through mother liquor circulation-dynamic carbonization |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2183584C1 (en) * | 2001-02-21 | 2002-06-20 | Государственное унитарное предприятие комбинат "Электрохимприбор" | Method of producing magnesium oxide |
| CN1539774A (en) * | 2003-10-31 | 2004-10-27 | 清华大学 | Method for preparing Nano magnesia from calcining light burning powder of magnesite |
| CN100333998C (en) * | 2005-12-07 | 2007-08-29 | 华东师范大学 | Method for preparing ultrafine nano-magnesia |
-
2007
- 2007-07-26 CN CN2007101375211A patent/CN101353176B/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948299A (en) * | 2010-09-14 | 2011-01-19 | 西南科技大学 | Preparation method of compact magnesia ceramics by sintering |
| CN105050955A (en) * | 2013-03-25 | 2015-11-11 | 神岛化学工业株式会社 | Magnesium oxide particles, resin composition, rubber composition, and molded article |
| CN105776255A (en) * | 2014-11-25 | 2016-07-20 | 重庆文理学院 | Preparation method of spherical magnesium oxide particles with large specific surface area |
| CN104495881B (en) * | 2014-12-19 | 2017-01-04 | 中南大学 | A kind of technique being prepared high-purity silicon-steel grade magnesium oxide by magnesium hydroxide |
| CN104495881A (en) * | 2014-12-19 | 2015-04-08 | 中南大学 | Process for preparing high-purity silicon steel magnesium oxide from magnesium hydroxide |
| CN105271319A (en) * | 2015-10-28 | 2016-01-27 | 内江师范学院 | Method for preparing nanometer MgO |
| CN105271318A (en) * | 2015-11-23 | 2016-01-27 | 中国科学院青海盐湖研究所 | Preparation method of magnesium oxide nanocrystalline |
| CN108569712A (en) * | 2018-04-04 | 2018-09-25 | 内江师范学院 | Preparation method of tetragonal body shape magnesium oxide material and products thereof and application |
| CN111848161A (en) * | 2020-08-05 | 2020-10-30 | 上海大学(浙江·嘉兴)新兴产业研究院 | Preparation method of nano zirconia powder |
| CN111848161B (en) * | 2020-08-05 | 2022-12-23 | 上海大学(浙江·嘉兴)新兴产业研究院 | Preparation method of nano zirconia powder |
| CN113184883A (en) * | 2021-05-11 | 2021-07-30 | 青海施丹弗化工有限责任公司 | Method for continuously producing nano magnesium oxide |
| CN114408950A (en) * | 2022-02-22 | 2022-04-29 | 上海太洋科技有限公司 | Supported high-dispersion nano magnesium oxide and preparation method and application thereof |
| CN114408950B (en) * | 2022-02-22 | 2023-08-29 | 上海太洋科技有限公司 | Supported high-dispersion nano magnesium oxide and preparation method and application thereof |
| CN115784275A (en) * | 2022-11-29 | 2023-03-14 | 中南大学 | Green method for preparing high-purity light magnesium oxide through mother liquor circulation-dynamic carbonization |
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| CN101353176B (en) | 2010-10-06 |
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