CN100391845C - Method for preparing nano-magnesia by utilizing self-spreading sol-gel method - Google Patents
Method for preparing nano-magnesia by utilizing self-spreading sol-gel method Download PDFInfo
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- CN100391845C CN100391845C CNB2005101111996A CN200510111199A CN100391845C CN 100391845 C CN100391845 C CN 100391845C CN B2005101111996 A CNB2005101111996 A CN B2005101111996A CN 200510111199 A CN200510111199 A CN 200510111199A CN 100391845 C CN100391845 C CN 100391845C
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Abstract
The present invention relates to a preparation method of nanometer magnesia, which is characterized in that the nanometer magnesia is prepared by using magnesium nitrate as a magensium source and apple acid, citric acid and triammonium citrate as complexing agents. The preparation method provided by the present invention has the advantages of low cost and easy acquirement of initial raw material, low requirement to equipment, low pollution to environment in the process of preparation, uniform particle size of the prepared nanometer material, no aggregation, good dispersivity, high purity, low calcination temperature, easy control of reaction, simple process operation and convenient realization of industrial production.
Description
Technical field
The present invention relates to a kind of method for preparing nano-magnesia by utilizing self-spreading sol-gel method of using, belong to the preparing technical field of nano magnesia.
Background technology
At present, preparation method for nanometer magnesium oxide is a lot, can be divided into solid phase method, vapor phase process, liquid phase method by the state of raw material.Solid phase method has mechanical crushing method, and this method requires very high to plant and instrument and is difficult to obtain particle less than 100 nanometers; The sample granularity of room temperature mechanochemical method preparation is inhomogeneous.Vapor phase process has physical vaporous deposition and chemical Vapor deposition process, and it is big to have throughput, advantages such as controllable granularity system, but product collection existing problems, and apparatus expensive, and energy consumption is big, and contaminate environment realizes that suitability for industrialized production also has certain difficulty.Liquid phase method is the method that extensively adopts at present, mainly contains direct precipitation method, sluggish precipitation, sol-gel method.Direct precipitation method, product granularity is big, broad particle distribution; Sluggish precipitation, the sedimentary uniform particles of gained and washing and filtering is convenient in densification, the product granularity that makes is little, narrowly distributing, reunion are few, and insufficient is that productivity ratio is lower; The nano-powder narrow particle size distribution that traditional sol-gel method makes, good dispersity, purity height, and calcining temperature is low, easy control of reaction system, and technological operation is simple, but raw materials cost is higher.
Summary of the invention
The objective of the invention is to release a kind of method for preparing nano-magnesia by utilizing self-spreading sol-gel method of using.
Technical scheme of the present invention is to be the magnesium source with the magnesium nitrate, with oxysuccinic acid, citric acid or ammonium citrate is complexing agent, magnesium nitrate and complexing agent are dissolved in the water, when complexing agent is oxysuccinic acid or citric acid, by the coordination of magnesium nitrate and complexing agent, with ammoniacal liquor regulator solution pH value to being not less than 4, when complexing agent is ammonium citrate, the pH value of regulator solution not then, through evaporation, dry, calcining, nano magnesia.
Now describe technical scheme of the present invention in detail.
A kind of method for preparing nano-magnesia by utilizing self-spreading sol-gel method of using is characterized in that,
The concrete operations step:
Producing of the first step presoma
Magnesium nitrate and complexing agent are dissolved in the water, the mol ratio of magnesium nitrate and complexing agent is 1: 1.5～4, and complexing agent is oxysuccinic acid, citric acid or ammonium citrate, when complexing agent is ammonium citrate, the pH value of regulator solution not then, when complexing agent is oxysuccinic acid or citric acid, with ammoniacal liquor regulator solution pH value to being not less than 4, evaporating solvent under 70 ℃～90 ℃ temperature, after getting gel, under 100 ℃～150 ℃ temperature, foam, get presoma, xerogel;
Producing of the second step nano magnesia
When complexing agent is citric acid or ammonium citrate, the presoma that the first step is made pre-burning 1.5 hours under 350 ℃ temperature earlier, again at the temperature lower calcination that is not less than 600 ℃, time is no less than 3 hours, when complexing agent is oxysuccinic acid, the presoma that the first step is made is at the temperature lower calcination that is not less than 600 ℃, and the time is no less than 3 hours, nano magnesia.
Compared with prior art, the present invention has following advantage:
1. raw material cheaply is easy to get, and method is simple, so preparation cost is lower.
2. reaction conditions gentleness, processing ease, to equipment require lowly, be convenient to realize industrialization.
3. preparation process is little to environment and people's pollution, belongs to green preparation process.
4. the little and granularity of product particle diameter is divided evenly, no agglomeration, and specific surface is big.
Embodiment
Embodiment 1
Complexing agent is an oxysuccinic acid.Get 1.2821g magnesium nitrate and 1.0057g oxysuccinic acid, promptly the mol ratio of magnesium nitrate and oxysuccinic acid is 1: 1.5, and it is dropped in the 20ml water, stirs it is dissolved fully.The pH value to 4 of ammoniacal liquor regulator solution stirred under the room temperature 1～2 hour.Solution is stirred evaporating solvent under 80 ℃ temperature, get gel.Gel is placed in the vacuum drying oven vacuum-drying 3h under 120 ℃ the temperature, presoma, xerogel.Calcining is 600 ℃ temperature lower calcination 3 hours, presoma generation self-propagating combustion during the calcining, temperature is 220 ℃, product, making the nano magnesia quality is 0.1685g.
Embodiment 2
Complexing agent is a citric acid.Get magnesium nitrate hexahydrate 2.0533g and be dissolved in the 20ml water, the strength of solution that is made into is 0.4mol/l, and citric acid is added magnesium nitrate solution, the mol ratio of magnesium nitrate and citric acid is 1: 4, the pH value to 4 of ammoniacal liquor regulator solution stirs evaporating solvent with solution under 80 ℃ temperature, get gel.Gel is placed in the vacuum drying oven vacuum-drying 3h under 120 ℃ the temperature, presoma, xerogel.Adopt substep thermal treatment, earlier with presoma pre-burning 1.5 hours under 350 ℃ temperature, presoma generation self-propagating combustion during the pre-burning, temperature is 180 ℃, to be placed on 600 ℃ temperature lower calcination 3 hours again through the presoma that pre-burning is handled, making the nano magnesia quality is 0.2572g.
Embodiment 3
Complexing agent is an ammonium citrate.Get magnesium nitrate hexahydrate 1.2821g and be dissolved in 20ml water, the strength of solution that is made into is 0.25mol/l, and ammonium citrate is added magnesium nitrate solution, and the mol ratio of magnesium nitrate and ammonium citrate is 1: 4.Stir evaporating solvent under the temperature with 80 ℃ of solution, get gel.Gel is placed in the vacuum drying oven vacuum-drying 3h under 120 ℃ the temperature, presoma, xerogel.Adopt substep thermal treatment, earlier with presoma pre-burning 1.5 hours under 350 ℃ temperature, presoma generation self-propagating combustion during the pre-burning, temperature is 180 ℃, to be placed on 600 ℃ of calcinings 3 hours again through the presoma that pre-burning is handled, making the nano magnesia quality is 0.1518g.
The nano magnesia that is made by aforesaid method is structure in the form of sheets, and particle diameter is little, even particle size distribution, and specific surface area is big.
Nano magnesia of many uses.Adopt nano magnesia, do not use sintering aid, just can realize low-temperature sintering, make the thin brilliant pottery of high-compactness, be expected to be developed as the tip materials of using under the severe condition such as high temperature, high corrosive environment.Nano magnesia 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.In addition, nano magnesia can be used as the filler of paint, paper and makeup, the additive of plastics and rubber and strengthening agent, the decomposition agent of fat, the polish of pharmaceuticals, chemosorbent, and the subsidiary material of various electronic material, catalyzer, superconductor, refractory materials etc.
Claims (2)
1. use method for preparing nano-magnesia by utilizing self-spreading sol-gel method for one kind, it is characterized in that, be the magnesium source with the magnesium nitrate, is complexing agent with oxysuccinic acid, citric acid or ammonium citrate, magnesium nitrate and complexing agent are dissolved in the water, when complexing agent is oxysuccinic acid or citric acid, by the coordination of magnesium nitrate and complexing agent, with ammoniacal liquor regulator solution pH value to being not less than 4, when complexing agent is ammonium citrate, the pH value of regulator solution not then, through evaporation, dry, calcining, nano magnesia.
2. the method for preparing nano-magnesia by utilizing self-spreading sol-gel method of using according to claim 1 is characterized in that the concrete operations step:
Producing of the first step presoma
Magnesium nitrate and complexing agent are dissolved in the water, the mol ratio of magnesium nitrate and complexing agent is 1: 1.5～4, and complexing agent is oxysuccinic acid, citric acid or ammonium citrate, when complexing agent is ammonium citrate, the pH value of regulator solution not then, when complexing agent is oxysuccinic acid or citric acid, with ammoniacal liquor regulator solution pH value to being not less than 4, evaporating solvent under 70 ℃～90 ℃ temperature, after getting gel, under 100 ℃～150 ℃ temperature, foam, get presoma, xerogel;
Producing of the second step nano magnesia
When complexing agent is citric acid or ammonium citrate, the presoma that the first step is made pre-burning 1.5 hours under 350 ℃ temperature earlier, again at the temperature lower calcination that is not less than 600 ℃, time is no less than 3 hours, when complexing agent is oxysuccinic acid, the presoma that the first step is made is at the temperature lower calcination that is not less than 600 ℃, and the time is no less than 3 hours, nano magnesia.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447305C (en) * | 2006-07-14 | 2008-12-31 | 西南大学 | Method for preparing magnesium oxide anti-corrosion protective film by sol-gel technology |
| CN100460061C (en) * | 2007-04-06 | 2009-02-11 | 华东师范大学 | Method for preparing nano-Ce-Magnesium coumpoud oxide |
| CN101269971B (en) * | 2007-08-06 | 2012-09-12 | 深圳市德方纳米科技有限公司 | Method of preparing nano-particle |
| CN100546914C (en) * | 2007-12-31 | 2009-10-07 | 浙江工业大学 | A kind of sol-gel self-propagating burning preparation CaIn 2O 4The method of powder |
| CN101279758B (en) * | 2008-05-16 | 2010-06-02 | 西北师范大学 | Preparation of nano-cupric oxide powder |
| CN108996530B (en) * | 2018-08-16 | 2020-09-22 | 军事科学院系统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 |
| CN109111230B (en) * | 2018-10-31 | 2020-12-29 | 航天特种材料及工艺技术研究所 | Yttrium oxide-magnesium oxide nano composite powder and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539774A (en) * | 2003-10-31 | 2004-10-27 | 清华大学 | Method for preparing Nano magnesia from calcining light burning powder of magnesite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1539774A (en) * | 2003-10-31 | 2004-10-27 | 清华大学 | Method for preparing Nano magnesia from calcining light burning powder of magnesite |
Non-Patent Citations (4)
| Title |
|---|
| "溶胶-凝胶法制备纳米氧化镁". 张志刚等.硅酸盐学报，第33卷第8期. 2005 |
| "溶胶-凝胶法制备纳米氧化镁研究". 宋士涛等.盐湖研究，第13卷第3期. 2005 |
| "溶胶-凝胶法制备纳米氧化镁". 张志刚等.硅酸盐学报，第33卷第8期. 2005 * |
| "溶胶-凝胶法制备纳米氧化镁研究". 宋士涛等.盐湖研究，第13卷第3期. 2005 * |
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