CN1207206C - Method for preparing nano magnesium oxide - Google Patents
Method for preparing nano magnesium oxide Download PDFInfo
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- CN1207206C CN1207206C CN 02155467 CN02155467A CN1207206C CN 1207206 C CN1207206 C CN 1207206C CN 02155467 CN02155467 CN 02155467 CN 02155467 A CN02155467 A CN 02155467A CN 1207206 C CN1207206 C CN 1207206C
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- magnesium
- solution
- magnesia
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Abstract
The present invention discloses a preparation method for nanometer level magnesia. In the method, soluble magnesium salt, sodium hydrate and a basic magnesium carbonate precipitant are used as raw materials so as to firstly manufacture a precursor of basic magnesium carbonate, and nanometer level magnesia powder is obtained by gradual temperature raise and calcining. The method has the advantages of simple and feasible technology, low preparation cost of the product, and easy realization of industrial production, and overcomes the defects of high cost of raw materials and production, complicated technology, high grain diameter of the manufactured magnesia, wide dispersion, etc. of the original preparation method. The obtained product has the grain diameter of 7 nm to 100 nm, narrow distribution, good dispersivity and high purity degree.
Description
Technical field:
The present invention relates to a kind of controllable method for preparing that all disperses the nano magnesia powder, belong to the preparation field of ceramic.
Background technology:
Nano magnesia is the novel high-performance fine inorganic material of a kind of particle diameter between 1～100nm, owing to its particle granular has the specific functions such as heat, light, electricity, mechanics and chemistry that are different from bulk material, all have been widely used in fields such as pottery, enamel, catalysis, weaving, medical science.Nano-powder magnesium oxide and superpolymer or other material are compounded with good microwave absorbing property, can be used as the packing material of makeup, paint, paper.Adopt the nano magnesia powder, need not use sintering aid just can realize low-temperature sintering, make high fine and close thin brilliant pottery, be expected to develop the tip materials under the severe condition such as high temperature, high corrosion.The nano magnesia powder also can be used as the sintering aid of other nanoparticles such as zirconium white, aluminum oxide, ferric oxide and stablizer and obtains high-quality nanophase pottery.
The preparation nano level method of magnesium oxide of bibliographical information is less relatively, generally is chemical process.Wherein more commonly vapor phase process, liquid phase method and sol-gel method.
Tokushi Kizuka (Materials Tansactions, JIM, 1998,39 (4): be raw material 508-514), adopt chemical vapor phase oxidation process, make the nano magnesia of sodium chloride type structure with the magnesium metal.The nano magnesia that this method makes, particle diameter are between 10-50nm, and crystal habit is more complete.(Journalof Physical Chemistry, 1994,98 (12): 3067-3070) described the new technology of laser vaporization/method of enrichment synthesizing nano-particle such as El-Shall M.S..The characteristics that this new technology can be controlled temperature and pressure in the advantage of pulse laser gasification and the scattering cloud chamber combine, and have synthesized multiple metal oxide and mixed metal oxide.This method can make the nano magnesia of 10-20nm.More than two kinds of method equipment expensive, production cost is high and be difficult for suitability for industrialized production.Open people (functional materials, 1999,30 (5): such as near, Wang Zhikui 557-558) with MgCl
26H
2O is a raw material, and slowly the dropping ammonia precipitation agent adopts direct precipitation method to make magnesium hydrate precipitate, and roasting obtains the nano magnesia powder.Adopt this method can make particle size range, the nano magnesia powder of average out to 62nm at 20-100nm.These method processing condition are wayward, the big and distribution range broad of the magnesium oxide powder particle diameter that makes.Open people (inorganic chemicals industry, 1999,31 (2): 3-5) in magnesium salt solution, add urea, make hydrolysis of urea discharge OH lentamente at a certain temperature such as near, Wang Guozhong
-Ion, control precipitation agent generating rate is limited in the proper range degree of supersaturation, thereby reaches control particle growth speed, and precipitation from homogeneous solution obtains even-grained presoma, and roasting obtains particle diameter at 24-39nm, the nano magnesia powder of average 30nm.This method technology is simpler relatively, and processing ease can make the nano magnesia powder that particle diameter is less, be evenly distributed.But because the hydrolysis of urea will be carried out in encloses container, so reaction vessel is had certain pressure requirement, equipment cost is higher.
Summary of the invention:
The objective of the invention is in order to overcome the shortcoming that the prior art for preparing nano magnesia exists, provide that a kind of cost is low, the nano magnesia powder preparation method of easy operation control.
The present invention is to be raw material with solubility magnesium salts and sodium hydroxide and soluble carbon hydrochlorate, makes the magnesium basic carbonate presoma earlier, obtains the nano magnesia powder of particle size range at 7～100nm through temperature-programmed calcination again.
Its concrete preparation method comprises the steps:
A. the solution that solubility divalence magnesium salts is made into 0.1～4.0mol/L adds reaction vessel, and the sodium hydroxide solution that drips concentration under the room temperature and be 0.1～20mol/L obtains white emulsion, and the dripping quantity of sodium hydroxide solution is pressed Mg
2+/ OH
-=1.8～2.5: 1 molar ratio computing, then with the soluble carbon hydrochlorate by with solution in Mg
2+Mol ratio be Mg
2+/ CO
3 2-=1: 1～1.5 ratio is poured reactor into, is warming up to 60 ℃～90 ℃, with 600～2500 rev/mins of stirring velocity stirring reaction 0.5～2h, the emulsion that obtains is chilled to room temperature, filters, washs, and promptly gets the magnesium basic carbonate presoma after 70 ℃～90 ℃ dryings.
Wherein the solubility magnesium salts can be: MgCl
2, MgBr
2, Mg (NO
3)
2, MgSO
4In any; The soluble carbon hydrochlorate can be: (NH
4)
2CO
3, NH
4HCO
3, Na
2CO
3In any.
B. with the magnesium basic carbonate presoma of above-mentioned preparation, under 550 ℃～950 ℃ temperature,, obtain the nano magnesia powder with temperature rise rate roasting 1～5h of 5～20 ℃/min.
The reactor that is adopted is the conversion unit of band heating commonly used and stirring; The roasting apparatus that is adopted is the electric heating roasting device, is not subjected to contaminating impurity to guarantee the roasting process material.
The magnesium oxide powder that obtains is carried out transmission electron microscope (TEM) analyzes, as a result its particle diameter all between 7～100nm, and narrowly distributing, good dispersity.Record this magnesium oxide powder specific surface area with the BET method and reach 46.7～160.9m
2/ g records purity with chemical titration and reaches more than 99%.
The present invention has adopted a kind of simple and easy to do method to prepare nano level magnesium oxide, and the product preparation cost is low, products obtained therefrom narrow diameter distribution, good dispersity, purity height.This preparation method is easy to realize suitability for industrialized production, and can reach controlled production to size and size-grade distribution by factors such as control reactant concn, proportioning, reaction times, presoma roasting conditions.
Description of drawings
Accompanying drawing 1 is the transmission electron microscope photo of the nano magnesia sample of the present invention's preparation, and as can be seen from the figure, the magnesium oxide powder particle diameter is between 7～25nm, and narrowly distributing, is uniformly dispersed.
Embodiment:
Embodiment 1: be the MgCl of 1.0mol/L with concentration
2Solution adds in the reaction vessel, and adding concentration under the room temperature is the NaOH solution (Mg of 5.0mol/L
2+/ OH
-=1.8: 1), obtain white emulsion, then with NH
4HCO
3Powder (Mg
2+/ CO
3 2-=1: 1.2) pour reactor into, be warming up to 60 ℃, with 800 rev/mins of stirring reaction 2h of stirring velocity.The emulsion that obtains is chilled to room temperature, and washing is to there not being Cl
-, promptly get the magnesium basic carbonate presoma after 3 hours in 70 ℃ of dryings.Roasting 1h after being warming up to 550 ℃ with the temperature rise rate of 10 ℃/min obtains magnesium oxide powder.Its particle diameter is in 10～20nm scope after measured, and specific surface area reaches 160.9m
2/ g, purity reaches 99.0%.
Embodiment 2: be the MgSO of 4.0mol/L with concentration
4Solution adds in the reaction vessel, and adding concentration under the room temperature is the NaOH solution (Mg of 20.0mol/L
2+/ OH
-=2.0: 1), obtain white emulsion, then with (NH
4)
2CO
3(Mg
2+/ CO
3 2-=1: 1.0) powder is poured reactor into, is warming up to 70 ℃, with 2000 rev/mins stirring velocity, and stirring reaction 30min.The emulsion that obtains is chilled to room temperature, and washing is to there not being SO
4 2-, promptly get the magnesium basic carbonate presoma after 2.5 hours in 80 ℃ of dryings.Roasting 1h after being warming up to 950 ℃ with the temperature rise rate of 15 ℃/min obtains magnesium oxide powder.Measure its particle diameter in 20～40nm scope through TEM, specific surface area is 35.1m
2/ g, purity reaches 99.4%.
Embodiment 3: be the Mg (NO of 0.2mol/L with concentration
3)
2Solution adds in the reaction vessel, and adding concentration under the room temperature is the NaOH solution (Mg of 5.0mol/L
2+/ OH
-)=2.2: 1), obtain white emulsion, then with NH
4HCO
3(Mg
2+/ HCO
3 -=1: 1.5) powder is poured reactor into, is warming up to 80 ℃, with 1800 rev/mins stirring velocity, and stirring reaction 1h.The emulsion that obtains is chilled to room temperature, and washing promptly gets the magnesium basic carbonate presoma in 90 ℃ of dryings after 2 hours.Roasting 2h after rising to 650 ℃ with the temperature rise rate of 10 ℃/min obtains magnesium oxide powder.Measure its particle diameter in 16～33nm scope through TEM, specific surface area reaches 122.4m
2/ g, purity reaches 99.5%.
Embodiment 4: be the MgCl of 4.0mol/L with concentration
2Solution adds in the reaction vessel, and adding concentration under the room temperature is the NaOH solution (Mg of 5.0mol/L
2+/ OH
-=2.5: 1), obtain white emulsion, then with Na
2CO
3Powder (Mg
2+/ CO
3 2-=1: 1.4) pour reactor into, be warming up to 60 ℃, with 1000 rev/mins stirring velocity stirring reaction 2h.The emulsion that obtains is chilled to room temperature, and washing is to there not being Cl
-, promptly get the magnesium basic carbonate presoma after 3 hours in 80 ℃ of dryings.Temperature rise rate with 20 ℃/min rises to 650 ℃ of roasting 1h, obtains the nano magnesia powder.Measure its particle diameter in 15～30nm scope through TEM, specific surface area reaches 133.4m
2/ g, purity reaches 99.1%.
Claims (2)
1. nanometer preparation process of magnesia, its concrete preparation process is as follows:
A. the solution that solubility divalence magnesium salts is made into 0.1～4.0mol/L adds reaction vessel, and the sodium hydroxide solution that drips concentration under the room temperature and be 0.1～20mol/L obtains white emulsion, and the dripping quantity of sodium hydroxide solution is pressed Mg
2+/ OH
-=1.8～2.5: 1 molar ratio computing, then with the soluble carbon hydrochlorate by with solution in Mg
2+Mol ratio be Mg
2+/ CO
3 2-=1: 1～1.5 ratio is poured reactor into, is warming up to 60 ℃～90 ℃, with 600～2500 rev/mins of stirring velocity stirring reaction 0.5～2h, the emulsion that obtains is chilled to room temperature, filters, washs, and promptly gets the magnesium basic carbonate presoma after 70 ℃～90 ℃ dryings;
B. with the magnesium basic carbonate presoma of steps A preparation, rise to roasting 1～5h after 550 ℃～950 ℃ temperature with the temperature rise rate of 5～20 ℃/min, obtain the nano magnesia powder.
2. preparation method according to claim 1, used solubility magnesium salts is: MgCl
2, MgBr
2, Mg (NO
3)
2, MgSO
4In any; Used soluble carbon hydrochlorate is: (NH
4)
2CO
3, NH
4HCO
3, Na
2CO
3In any.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02155467 CN1207206C (en) | 2002-12-13 | 2002-12-13 | Method for preparing nano magnesium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02155467 CN1207206C (en) | 2002-12-13 | 2002-12-13 | Method for preparing nano magnesium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1508072A CN1508072A (en) | 2004-06-30 |
| CN1207206C true CN1207206C (en) | 2005-06-22 |
Family
ID=34235920
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02155467 Expired - Fee Related CN1207206C (en) | 2002-12-13 | 2002-12-13 | Method for preparing nano magnesium oxide |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299992C (en) * | 2005-09-06 | 2007-02-14 | 山东大学 | High purity magnesium oxide cleaning production method |
| CN1331984C (en) * | 2006-02-23 | 2007-08-15 | 山东大学 | Prepn of magnesium hydroxide for fire retardant |
| SI2322581T1 (en) * | 2009-11-03 | 2015-10-30 | Omya International Ag | Process for preparing hydromagnesite |
| US9061920B2 (en) | 2009-11-10 | 2015-06-23 | Omya International Ag | Precipitated magnesium carbonate |
| CN101993099B (en) * | 2010-12-09 | 2013-07-24 | 深圳市华力兴工程塑料有限公司 | Nano magnesium carbonate crystal and preparation method thereof |
| CN102942198B (en) * | 2012-10-16 | 2016-04-20 | 桐柏兴源化工有限公司 | A kind of Method of Soda produces the method for low chlorine high-purity magnesium oxide |
| CN104445304A (en) * | 2014-12-09 | 2015-03-25 | 天津渤化永利化工股份有限公司 | Method for preparing basic magnesium carbonate by using combinative alkali system high-salt heavy-ash mother solution |
| CN104607142B (en) * | 2015-01-20 | 2017-09-15 | 中国科学院合肥物质科学研究院 | Micro-nano hierarchy MgO/MgCO3Compound and its application as defluorinating agent |
| CN105271319B (en) * | 2015-10-28 | 2017-01-18 | 内江师范学院 | Method for preparing nanometer MgO |
| CN105312151A (en) * | 2015-12-14 | 2016-02-10 | 苏州市泽镁新材料科技有限公司 | Magnesium oxide impurity removing process |
| CN107142490B (en) * | 2017-05-10 | 2019-04-26 | 东北大学 | A kind of magnesium chloride electrotransformation is the method for high-purity magnesium oxide |
| CN108996530B (en) * | 2018-08-16 | 2020-09-22 | 军事科学院***工程研究院卫勤保障技术研究所 | Preparation method of nano magnesium oxide, nano magnesium oxide-nano fiber composite felt, and preparation method and application thereof |
| 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 |
| CN115814752B (en) * | 2023-01-31 | 2024-04-05 | 成都理工大学 | Composite material of calcium carbonate and nano magnesium oxide and preparation and application methods thereof |
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2002
- 2002-12-13 CN CN 02155467 patent/CN1207206C/en not_active Expired - Fee Related
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