CN101850993A - Preparation method of rodlike nanometer magnesium oxide - Google Patents
Preparation method of rodlike nanometer magnesium oxide Download PDFInfo
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- CN101850993A CN101850993A CN 201010199975 CN201010199975A CN101850993A CN 101850993 A CN101850993 A CN 101850993A CN 201010199975 CN201010199975 CN 201010199975 CN 201010199975 A CN201010199975 A CN 201010199975A CN 101850993 A CN101850993 A CN 101850993A
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Abstract
The invention relates to a preparation method of rodlike nanometer magnesium oxide, belonging to the technical field of materials. The preparation method comprises the following steps of: (1) dissolving soluble magnesium salt, sodium hydroxide as a precipitator and a crystal form controlling agent into water as raw materials to prepare a reaction solution, wherein the crystal form controlling agent is glycol, starch, emulsifier OP10 or triethanolamine; and (2) reacting the prepared reaction solution for 20-40 minutes under a stirring condition with the temperature of 20-90 DEG C to obtain a deposition as a precursor; and (3) calcining the obtained precursor for 2-4h under 550-750 DEG C. In the invention, the incompact precursor is obtained through selecting the crystal form controlling agent and controlling the deposition condition, and the calcining condition is controlled to prepare the rodlike nanometer magnesium oxide. The obtained rodlike nanometer magnesium oxide has controllable grain diameter and draw ratio. The method has the advantages of easily obtained raw materials, simple process, suitability for industrial production, and the like, and has good application prospect in the technical field of infrared stealth materials.
Description
Technical field
The invention belongs to the material technology field, particularly a kind of preparation method of rodlike nanometer magnesium oxide.
Background technology
Nano magnesia is a kind of novel high function fine inorganic material, except having common magnesian character and purposes, because particle enters nanoscale, make nano magnesia because of outside the common surface effects of nanoparticle, quantum size effect, volume effect, the macro quanta tunnel effect, but also have the not available character of a series of common magnesium oxide, thereby a series of new Application Areass have been opened up.Nano magnesia has properties such as the heat that is different from bulk material, light, electricity, mechanics, chemistry, industrial important application prospects and huge economic potential is arranged.Infrared absorption is a kind of of stealthy technique, and the infrared stealth material is a focus of current stealthy technique research, has wide research prospect.
The preparation of nano magnesia at present has several different methods, in recent years result of study shows, adopts solubility magnesium salts and precipitant mix, again by tensio-active agent control grain shape, under stirring, ultrasonic wave or heating condition, make precipitation, obtain nano magnesia through calcining then.The morphology control of nanometer is mainly by reaction times, temperature of reaction, agitation condition and calcining temperature and time decision in the existing method, tensio-active agent of selecting for use such as stearate etc. cost higher, the more important thing is the effect that achieves no breakthrough of vpg connection at the control nano magnesia; Difform nano magnesia has different characteristic infrared absorptions, be applicable to various infrared absorbance range, how to select subsidiary material such as tensio-active agent preferably, and determine other processing condition according to different materials, preparing nano oxidized magnesium material controllable shapes, that be fit to particular requirement is present urgent problem.
Summary of the invention
At the deficiency that exists on the existing nano magnesia technology of preparing, the invention provides a kind of preparation method of rodlike nanometer magnesium oxide, purpose is by the crystal formation control agent of selecting to suit, and determines the operational path of optimization, adopts low cost and the simple method of technology to prepare rod-like nano magnesium oxide.
Method of the present invention is carried out according to the following steps:
1, solubility magnesium salts, precipitation agent sodium hydroxide and crystal formation control agent is soluble in water as reaction raw materials, make reaction soln, the composition of reaction raw materials is sodium hydroxide 27～44% by weight percentage, solubility magnesium salts 55～72%, crystal formation control agent 0.1～2%, the consumption of water is to be as the criterion whole material dissolutions; Described crystal formation control agent is ethylene glycol, starch, polyoxyethylene nonylphenol ether 10 or trolamine.
2, reaction soln is reacted 20～40min under 20～90 ℃ and agitation condition, stirring velocity is 200～900rpm, acquisition be precipitated as presoma.
3, the presoma that obtains is calcined 2～4h under 550～750 ℃ of conditions, obtain rod-like nano magnesium oxide.
Above-mentioned solubility magnesium salts is magnesium chloride or magnesium nitrate.
The magnesian length-to-diameter ratio of above-mentioned rod-like nano is 1.26～1.42, and length is 38～75nm, and diameter is 27～53nm.
Method of the present invention obtains loose presoma by the control deposition condition simultaneously by choosing ethylene glycol, starch, polyoxyethylene nonylphenol ether 10 or trolamine as the crystal formation control agent, makes rod-like nano magnesium oxide by the control calcination condition again; The rod-like nano magnesium oxide particle diameter and the length-to-diameter ratio that obtain are controlled.Method of the present invention has raw material and is easy to get, and technology is simple, is applicable to advantages such as suitability for industrialized production, has a good application prospect in infrared stealth material technology field.
Description of drawings
Fig. 1 is the magnesian TEM figure of the rod-like nano of the embodiment of the invention 1.
Fig. 2 is the magnesian TEM figure of the rod-like nano of the embodiment of the invention 2.
Fig. 3 is the magnesian XRD figure of the rod-like nano of the embodiment of the invention 1.
Fig. 4 is the magnesian characteristic infrared absorption figure of the rod-like nano of the embodiment of the invention 1.
Embodiment
Magnesium chloride that adopts in the embodiment of the invention and magnesium nitrate are technical grade product.
The ethylene glycol that adopts in the embodiment of the invention, starch, polyoxyethylene nonylphenol ether 10 and trolamine are technical grade product.
The calciner that adopts in the embodiment of the invention is a retort furnace.
Embodiment 1
Magnesium chloride, sodium hydroxide and crystal formation control agent ethylene glycol is soluble in water as reaction raw materials, make reaction soln, the weight percent of sodium hydroxide is 27% in the reaction raw materials, the weight percent of magnesium salts is 72%, the weight percent of crystal formation control agent is 1%, and the consumption of water is to be as the criterion whole material dissolutions.
With reaction soln stirring reaction 40min under 20 ℃ of conditions, stirring velocity is 900rpm, filters then throw out and aqueous phase separation.
The throw out that obtains is calcined 4h under 550 ℃ of conditions, obtain rod-like nano magnesium oxide.
The magnesian length-to-diameter ratio of rod-like nano is 1.26, and length is 48nm, and diameter is 38nm.
The magnesian TEM figure of rod-like nano as shown in Figure 1.
Adopt X-ray diffraction method (XRD) to calculate the nano magnesia grain diameter.Test gained sample is by the X ' Pert Pro type x-ray diffractometer detection of Dutch PANalytical company, and XRD can provide the data of nano material grain-size easily.Be based on relevant this phenomenon of width of diffraction peak with grain-size with the principle of XRD measurement nano material grain-size size.When grain-size during less than 100nm, its diffraction peak width is changed significantly with grain size, and grain size can adopt the Scherrer formula to calculate:
D＝Kλ/B
1/2cosθ
In the formula, D is for also can think the grain-size size along the thickness of crystal face vertical direction, and K is the Scherrer constant of diffraction peak shape, generally gets 0.89, and λ is the wavelength of ray, B
1/2Be the halfwidth of diffraction peak, θ is the Bragg diffraction angle.
The magnesian XRD figure of rod-like nano as shown in Figure 3; Characteristic infrared absorption as shown in Figure 4.
Embodiment 2
Magnesium nitrate, sodium hydroxide and crystal formation control agent starch is soluble in water as reaction raw materials, make reaction soln, the weight percent of sodium hydroxide is 44% in the reaction raw materials, the weight percent of magnesium salts is 55%, the weight percent of crystal formation control agent is 1%, and the consumption of water is to be as the criterion whole material dissolutions.
With reaction soln stirring reaction 20min under 90 ℃ of conditions, stirring velocity is 200rpm, filters then throw out and aqueous phase separation.
The throw out that obtains is calcined 3h under 600 ℃ of conditions, obtain rod-like nano magnesium oxide.
The magnesian length-to-diameter ratio of rod-like nano is 1.42, and length is 75nm, and diameter is 53nm.
The magnesian TEM figure of rod-like nano as shown in Figure 2.
Embodiment 3
Magnesium chloride, sodium hydroxide and crystal formation control agent polyoxyethylene nonylphenol ether 10 is soluble in water as reaction raw materials, make reaction soln, the weight percent of sodium hydroxide is 39.5% in the reaction raw materials, the weight percent of magnesium salts is 60.4%, the weight percent of crystal formation control agent is 0.1%, and the consumption of water is to be as the criterion whole material dissolutions.
With reaction soln stirring reaction 30min under 50 ℃ of conditions, stirring velocity is 600rpm, filters then throw out and aqueous phase separation.
The throw out that obtains is calcined 3h under 700 ℃ of conditions, obtain rod-like nano magnesium oxide.
The magnesian length-to-diameter ratio of rod-like nano is 1.41, and length is 38nm, and diameter is 27nm.
Embodiment 4
Magnesium nitrate, sodium hydroxide and crystal formation control agent trolamine is soluble in water as reaction raw materials, make reaction soln, the weight percent of sodium hydroxide is 35% in the reaction raw materials, the weight percent of magnesium salts is 63%, the weight percent of crystal formation control agent is 2%, and the consumption of water is to be as the criterion whole material dissolutions.
With reaction soln stirring reaction 30min under 60 ℃ of conditions, stirring velocity is 400rpm, filters then throw out and aqueous phase separation.
The throw out that obtains is calcined 2h under 750 ℃ of conditions, obtain rod-like nano magnesium oxide.
The magnesian length-to-diameter ratio of rod-like nano is 1.38, and length is 58nm, and diameter is 42nm.
Claims (3)
1. preparation method of rodlike nanometer magnesium oxide is characterized in that carrying out according to the following steps:
(1) solubility magnesium salts, precipitation agent sodium hydroxide and crystal formation control agent is soluble in water as reaction raw materials, make reaction soln, the composition of reaction raw materials is sodium hydroxide 27～44% by weight percentage, solubility magnesium salts 55～72%, crystal formation control agent 0.1～2%, the consumption of water is to be as the criterion whole material dissolutions; Described crystal formation control agent is ethylene glycol, starch, polyoxyethylene nonylphenol ether 10 or trolamine;
(2) reaction soln made is reacted 20～40min under 20～90 ℃ and agitation condition, stirring velocity is 200～900rpm, acquisition be precipitated as presoma;
(3) presoma that obtains is calcined 2～4h under 550～750 ℃ of conditions, obtain rod-like nano magnesium oxide.
2. a kind of preparation method of rodlike nanometer magnesium oxide according to claim 1 is characterized in that described solubility magnesium salts is magnesium chloride or magnesium nitrate.
3. a kind of preparation method of rodlike nanometer magnesium oxide according to claim 1 is characterized in that described rod-like nano magnesium oxide length-to-diameter ratio is 1.26～1.42, and length is 38～75nm, and diameter is 27～53nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106673590A (en) * | 2016-09-13 | 2017-05-17 | 内蒙古博大新型墙体材料研究所 | Novel heat preservation and isolation wall body material and preparation method thereof |
| CN112897559A (en) * | 2021-02-26 | 2021-06-04 | 绵阳远达电子材料有限公司 | Production process of magnesium hydroxide |
| CN113416592A (en) * | 2021-05-24 | 2021-09-21 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
-
2010
- 2010-06-13 CN CN2010101999753A patent/CN101850993B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 《中国粉体技术》 20090331 王小宇等 菱镁矿为原料制备纳米氧化镁粉体的工艺研究 第49页，1.2 试验方法，第52页2.3 纳米氧化镁的制备 1-3 第15卷, 2 * |
| 《科技资讯》 20071231 李宪平 均匀沉淀法制备纳米氧化镁的研究 第28页，2.4.2表面活性剂的选择和加入量的影响 1-3 , 第8期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106673590A (en) * | 2016-09-13 | 2017-05-17 | 内蒙古博大新型墙体材料研究所 | Novel heat preservation and isolation wall body material and preparation method thereof |
| CN112897559A (en) * | 2021-02-26 | 2021-06-04 | 绵阳远达电子材料有限公司 | Production process of magnesium hydroxide |
| CN113416592A (en) * | 2021-05-24 | 2021-09-21 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
| CN113416592B (en) * | 2021-05-24 | 2022-07-29 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
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| CN101850993B (en) | 2012-02-22 |
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