CN100486895C - Preparation method for nanometer magnesium oxide - Google Patents
Preparation method for nanometer magnesium oxide Download PDFInfo
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- CN100486895C CN100486895C CNB2007100391753A CN200710039175A CN100486895C CN 100486895 C CN100486895 C CN 100486895C CN B2007100391753 A CNB2007100391753 A CN B2007100391753A CN 200710039175 A CN200710039175 A CN 200710039175A CN 100486895 C CN100486895 C CN 100486895C
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Abstract
This invention relates to a preparation method for MgO nm crystals, which takes soluble Mg salt as the source and adds surface active agent in it, takes sodium oxalate as the deposition agent to heat-react in a high pressure kettle for a period of time then to take out the precursor to deposit, centrifuge and clean it to be dried at normal temperature in vacuum, then burns the dried precursor in a muffle for a period of time to produce MgO nm crystals.
Description
Technical field
The present invention relates to a kind of preparation method of bitter earth nano crystalline substance, belong to the nano material preparation technical field.
Background technology
Nano magnesia has properties such as the heat that is different from bulk material, light, electricity, mechanics, chemistry, adopt nano magnesia, do not use sintering aid just can realize low-temperature sintering, make high fine and close thin brilliant pottery, be expected to be developed as the tip materials under the severe condition such as high temperature, high corrosive environment; It 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 nano ceramics.Nano magnesia has good shielding ultraviolet rays performance, is the most preferably material of development functionality makeup, fiber and clothes.Nano magnesia also has good bacteriostatic activity and photocatalytic activity.It is widely used in fields such as advanced ceramic materials, insulating material, makeup, paint, rubber filler, sour gas sorbent material, support of the catalyst, and wide application prospect and huge economic potential are arranged.
The report for preparing about nano magnesia both at home and abroad has vapor phase process, sol-gel method, metal alkoxide hydrolysis method, direct precipitation method, sluggish precipitation, water-sol method, indoor temperature solid phase method etc. at present.More than these methods or to equipment and technical requirements is higher or processing condition control difficulty or raw materials cost height or yield poorly, limited producing and using of nano magnesia.
In the magnesian preparation of report, Hydrothermal Preparation mostly needs the reaction conditions of High Temperature High Pressure, so energy consumption is big, and is difficult to obtain super fine magnesia at present.
Summary of the invention
The object of the present invention is to provide a kind of high quality, low cost, less energy-consumption, the magnesian preparation of superfine nano.
Concrete operations of the present invention: with the solubility magnesium salts is the magnesium source, add tensio-active agent, with the sodium oxalate is precipitation agent, reaction soln is hydro-thermal reaction for some time in autoclave, take out presoma precipitation centrifuge washing vacuum Air drying, presoma in retort furnace calcination for some time good drying promptly makes the bitter earth nano crystal.It is the magnesium source that the present invention adopts magnesium chloride, makes it to be dissolved in the water, and adding disodium ethylene diamine tetraacetate again is tensio-active agent, mix, add the sodium oxalate mixing again, put into autoclave, making its compactedness is 60～80%, heats to make it to take place hydro-thermal reaction in 2～12 hours; Reaction finishes the back and takes out presoma precipitation centrifuge washing, and normal temperature vacuum-drying in vacuum drying oven is again heated calcination to dry precursor in retort furnace, and the calcination process is carried out in two steps, the first step: calcination is 1～2 hour between 350～450 ℃; Second step: be warmed up between 600～650 ℃ calcination 1～2 hour.Gained is the bitter earth nano crystal after finishing.By the bitter earth nano crystal particle diameter narrowly distributing that aforesaid method makes, degree of crystallinity height, particle diameter are between 5～10nm, and productive rate is more than 90%.
The present invention compares with existing preparation technology has advantage:
(1) reaction raw materials magnesium of the present invention source is a Magnesium dichloride hexahydrate, and the bittern resource of desirable China's abundant cheaply is easy to get, and has reduced production cost;
(2) hydrothermal temperature of the present invention is low, has reduced the consumption of the energy and to the requirement of equipment, has helped industrialization promotion;
(3) the present invention prepares nano magnesia crystal yield height, and product cut size is evenly distributed, and particle diameter is little, reaches 5～10nm.
Description of drawings
Fig. 1: be nano magnesia crystalline TEM figure and electron-diffraction diagram
Embodiment
Embodiment 1: get the 0.4855g magnesium chloride, at volume is with the 6ml water dissolution in the autoclave of 20ml, add 0.0179g disodium ethylene diamine tetraacetate stirring and evenly mixing wiring solution-forming A again, other takes by weighing the solution B that the 0.3126g sodium oxalate is made into 6ml, B is added mixing among the A under condition of stirring, issue unboiled water thermal response 10h at 160 ℃, centrifuge washing (checking with Silver Nitrate) till do not have chlorion obtains presoma behind the naturally cooling, vacuum Air drying 24h, the calcination in retort furnace of dried presoma, this process be in two steps: the first step: at 450 ℃ of calcination 1.5h; Second step: be warmed up to 600 ℃ of calcination 1.5h.Promptly obtain the nano oxidized magnesium crystal of white.
Embodiment 2: get the 1.2108g magnesium chloride, at volume is with the 7.5ml water dissolution in the autoclave of 20ml, add 0.0446g disodium ethylene diamine tetraacetate stirring and evenly mixing wiring solution-forming A again, other takes by weighing the solution B that the 0.8064g sodium oxalate is made into 7.5ml, B is added mixing among the A under condition of stirring, issue unboiled water thermal response 4h at 100 ℃, centrifuge washing (checking with Silver Nitrate) till do not have chlorion obtains presoma behind the naturally cooling, vacuum Air drying 24h, the calcination in retort furnace of dried presoma, this process be in two steps: the first step: at 400 ℃ of calcination 1h; Second step: be warmed up to 600 ℃ of calcination 2h.Promptly obtain the nano oxidized magnesium crystal of white.
Embodiment 3: get the 1.5248g magnesium chloride, at volume is with the 7ml water dissolution in the autoclave of 20ml, add 0.0559g disodium ethylene diamine tetraacetate stirring and evenly mixing wiring solution-forming A again, other takes by weighing the solution B that the 1.005g sodium oxalate is made into 7ml, B is added mixing among the A under condition of stirring, issue unboiled water thermal response 6h at 100 ℃, centrifuge washing (checking with Silver Nitrate) till do not have chlorion obtains presoma behind the naturally cooling, vacuum Air drying 24h, the calcination in retort furnace of dried presoma, this process be in two steps: the first step: at 450 ℃ of calcination 1.5h; Second step: be warmed up to 600 ℃ of calcination 1.5h.Promptly obtain the nano oxidized magnesium crystal of white.
Claims (2)
1. preparation method for nanometer magnesium oxide, it is characterized in that the solubility magnesium salts after water dissolution, add disodium ethylene diamine tetraacetate, add sodium oxalate again, mix, mixture is put into autoclave, make that the autoclave compactedness is 60%～80%, heating, temperature should be controlled between 100 ℃～180 ℃, make it to take place hydro-thermal reaction, reaction finishes the back and takes out presoma precipitation, centrifuge washing, after the normal temperature vacuum-drying, heat calcination in retort furnace, the calcination process is carried out in two steps, the first step: calcination is 1～2 hour between 350 ℃～450 ℃; Second step: be warmed up between 600 ℃～650 ℃ calcination 1～2 hour, and promptly got nano magnesia.
2. preparation method for nanometer magnesium oxide as claimed in claim 1 is characterized in that the solubility magnesium salts is a magnesium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100391753A CN100486895C (en) | 2007-04-06 | 2007-04-06 | Preparation method for nanometer magnesium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100391753A CN100486895C (en) | 2007-04-06 | 2007-04-06 | Preparation method for nanometer magnesium oxide |
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| Publication Number | Publication Date |
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| CN101033073A CN101033073A (en) | 2007-09-12 |
| CN100486895C true CN100486895C (en) | 2009-05-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2007100391753A Expired - Fee Related CN100486895C (en) | 2007-04-06 | 2007-04-06 | Preparation method for nanometer magnesium oxide |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265058B (en) * | 2013-05-20 | 2014-10-29 | 复旦大学 | Synthetic method of {111} crystal face preferred magnesium oxide material |
| CN104437628A (en) * | 2014-11-29 | 2015-03-25 | 南京威安新材料科技有限公司 | Catalyst production method |
| CN105366696A (en) * | 2015-12-14 | 2016-03-02 | 苏州市泽镁新材料科技有限公司 | Method for preparing high-purity nanometer magnesia |
| CN109422949A (en) * | 2017-09-05 | 2019-03-05 | 张家港市沐和新材料技术开发有限公司 | A kind of modified Nano magnesia-composite polyethylene material and preparation method thereof |
| CN109433183B (en) * | 2018-11-01 | 2021-09-03 | 河南科技学院 | Bimetal composite oxide catalyst, preparation method and application |
| CN115286022A (en) * | 2022-08-29 | 2022-11-04 | 长江师范学院 | Preparation method and application of MgO nano material for preventing and treating clubroot of tumorous stem mustard |
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2007
- 2007-04-06 CN CNB2007100391753A patent/CN100486895C/en not_active Expired - Fee Related
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| CN101033073A (en) | 2007-09-12 |
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Granted publication date: 20090513 Termination date: 20120406 |