CN101920977A - Preparation method of flaky nano-sized magnesium oxide - Google Patents
Preparation method of flaky nano-sized magnesium oxide Download PDFInfo
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- CN101920977A CN101920977A CN 201010246810 CN201010246810A CN101920977A CN 101920977 A CN101920977 A CN 101920977A CN 201010246810 CN201010246810 CN 201010246810 CN 201010246810 A CN201010246810 A CN 201010246810A CN 101920977 A CN101920977 A CN 101920977A
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Abstract
The invention relates to a preparation method of flaky nano-sized magnesium oxide, belonging to the technical field of materials. The preparation method comprises the following steps of: (1) adding soluble magnesium salt, organic dispersant and precipitant ammonia water into water, and carrying out precipitation reaction under the condition of stirring to obtain precipitate magnesium hydroxide precursor, wherein the reaction temperature is 40-50 DEG C, the stirring speed is 300-400rpm, and the reaction time is at least 60min; and (2) calcining the magnesium hydroxide precursor at 500-600 DEG C to obtain the flaky nano-sized magnesium oxide. The method of the invention has the advantages of easy acquisition of raw materials, simple processes and the like, is suitable for industrialized production, and has good application prospects in the technical field of infrared camouflage materials.
Description
Technical field
The invention belongs to the material technology field, particularly a kind of preparation method of flaky nano-sized 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
The invention provides a kind of preparation method of flaky nano-sized magnesium oxide, purpose is by selection magnesium salts, organic dispersing agent and precipitation agent, and the adjustment reaction conditions, prepares the flake nano magnesium oxide with unique characteristic infrared absorption.
Method of the present invention is carried out according to the following steps:
1, solubility magnesium salts, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of solubility magnesium salts and ammoniacal liquor is 1: 0.2～0.6, organic dispersing agent account for the solubility magnesium salts gross weight 2～4%, temperature of reaction is 40～50 ℃, stirring velocity is 300～400rpm, and the reaction times is 60min at least, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is one or more mixing in oxalic acid, trolamine, citric acid, EDTA, ethylene glycol, glycerol and the polyoxyethylene glycol.
2, the magnesium hydroxide presoma is calcined 1～3h under 500～600 ℃ of conditions, obtain flake nano magnesium oxide.
Above-mentioned solubility magnesium salts is sal epsom, magnesium nitrate or magnesium chloride.
The magnesian outward appearance of above-mentioned flake nano is a sheet, and thickness is at 13～36nm; The flake nano magnesium oxide of preparation is through being sheet with visible its outward appearance of transmission electron microscope or scanning electron microscopic observation.
Method of the present invention is mixed with ammoniacal liquor by selecting sal epsom, magnesium nitrate and magnesium chloride for use, carries out precipitin reaction under the condition that adds carboxyl class organic dispersing agent, and then calcining obtains flake nano magnesium oxide.The selection aspect of precipitation agent, ammoniacal liquor is weak base, constantly ionization goes out OH in water
-React the generation precipitation with magnesium ion, the nano magnesia of generation disperses in order; And adopt sodium hydroxide is precipitation agent, and the nano magnesia agglomeration of generation is more serious, and employing yellow soda ash is precipitation agent, and the magnesium oxide of generation is irregular shape, and portioned product exceeds the scope of nano material; On the adding mode of precipitation agent, when precipitation agent slowly splashed into, the product of acquisition was spherical, is sheet and adopt the product of the method acquisition of instantaneous adding simultaneously.The selection of organic dispersing agent mainly is carboxyl class or hydroxy kind organic reagent, carboxyl or hydroxyl quantity increase the granularity that can reduce nano oxidized magnesium products within the specific limits in the test discovery organic dispersing agent, descend when carboxyl quantity too much then can cause product lattice imperfection or granularity, adopt the organic dispersing agent of three carboxyls or tetracarboxylic can obtain flake nano magnesium oxide; In the hydroxy kind organic dispersing agent, along with hydroxyl quantity in the organic dispersing agent increases within the specific limits, nano oxidized magnesium products pattern is tending towards evenly complete, and when hydroxyl quantity was too much, its situation and carboxyl class organic dispersing agent were similar.
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 SEM figure of the flake nano in the embodiment of the invention 1.
Fig. 2 is the magnesian SEM figure of the flake nano in the embodiment of the invention 2.
Fig. 3 is the magnesian SEM figure of the flake nano in the embodiment of the invention 3.
Fig. 4 is the magnesian SEM figure of the flake nano in the embodiment of the invention 4.
Fig. 5 is the magnesian SEM figure of the flake nano in the embodiment of the invention 5.
Fig. 6 is the magnesian SEM figure of the flake nano in the embodiment of the invention 6.
Fig. 7 is the magnesian XRD figure of the flake nano in the embodiment of the invention 1.
Fig. 8 is the magnesian XRD figure of the flake nano in the embodiment of the invention 2.
Fig. 9 is the magnesian characteristic infrared absorption figure of flake nano that rod-like nano magnesium oxide and the present invention obtain, and a is a rod-like nano magnesium oxide among the figure, and b is a flake nano magnesium oxide.
Embodiment
The sal epsom that adopts in the embodiment of the invention, magnesium nitrate and ammoniacal liquor are analytical reagent.
The oxalic acid that adopts in the embodiment of the invention, trolamine, citric acid, EDTA, ethylene glycol, glycerol and polyoxyethylene glycol are analytical reagent.
The calciner that adopts in the embodiment of the invention is a retort furnace.
Embodiment 1
Magnesium chloride, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of magnesium salts and ammoniacal liquor is 1: 0.5, organic dispersing agent account for the solubility magnesium salts gross weight 3%, temperature of reaction is 40 ℃, stirring velocity is 300rpm, and the reaction times is 60min, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is the mixture of EDTA and polyoxyethylene glycol, and the quality proportioning is 1: 1.
The magnesium hydroxide presoma is calcined 2h under 550 ℃ of conditions, obtain flake nano magnesium oxide, outward appearance is a sheet, and the sheet mean thickness is 13nm.
Magnesium chloride, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of solubility magnesium salts and ammoniacal liquor is 1: 0.6, organic dispersing agent account for magnesium salts gross weight 4%, temperature of reaction is 60 ℃, stirring velocity is 300rpm, and the reaction times is 60min, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is the mixture of EDTA and trolamine, and the quality proportioning is 1: 1.
The magnesium hydroxide presoma is calcined 3h under 550 ℃ of conditions, obtain flake nano magnesium oxide, outward appearance is a sheet, and the sheet mean thickness is 36nm.
Embodiment 3
Sal epsom, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of solubility magnesium salts and ammoniacal liquor is 1: 0.2, organic dispersing agent account for magnesium salts gross weight 2%, temperature of reaction is 40 ℃, stirring velocity is 350rpm, and the reaction times is 70min, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is the mixture of EDTA and polyoxyethylene glycol, and the quality proportioning is 1: 1.
The magnesium hydroxide presoma is calcined 3h under 600 ℃ of conditions, obtain flake nano magnesium oxide, outward appearance is a sheet, and the sheet mean thickness is 26nm.
Embodiment 4
Sal epsom, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of solubility magnesium salts and ammoniacal liquor is 1: 0.3, organic dispersing agent account for magnesium salts gross weight 3%, temperature of reaction is 50 ℃, stirring velocity is 400rpm, and the reaction times is 60min, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is the mixture of citric acid and polyoxyethylene glycol, and the quality proportioning is 1: 1.
The magnesium hydroxide presoma is calcined 3h under 600 ℃ of conditions, obtain flake nano magnesium oxide, outward appearance is a sheet, and the sheet mean thickness is 29nm.
Embodiment 5
Magnesium nitrate, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of magnesium salts and ammoniacal liquor is 1: 0.3, organic dispersing agent account for magnesium salts gross weight 2.5%, temperature of reaction is 40 ℃, stirring velocity is 350rpm, and the reaction times is 60min, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is the mixture of citric acid and ethylene glycol, and the quality proportioning is 1: 1.
The magnesium hydroxide presoma is calcined 2h under 500 ℃ of conditions, obtain flake nano magnesium oxide, outward appearance is a sheet, and the sheet mean thickness is 13nm.
Magnesium nitrate, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of magnesium salts and ammoniacal liquor is 1: 0.4, organic dispersing agent account for magnesium salts gross weight 3%, temperature of reaction is 50 ℃, stirring velocity is 300rpm, and the reaction times is 65min, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is the mixture of citric acid, oxalic acid and glycerol, and the quality proportioning is 1: 1: 1.
The magnesium hydroxide presoma is calcined 2h under 500 ℃ of conditions, obtain flake nano magnesium oxide, outward appearance is a sheet, and the sheet mean thickness is 13nm.
Claims (3)
1. preparation method of flaky nano-sized magnesium oxide is characterized in that carrying out according to the following steps:
(1) solubility magnesium salts, organic dispersing agent and precipitation agent ammoniacal liquor are added in the entry, under agitation condition, carry out precipitin reaction, wherein the weight ratio of solubility magnesium salts and ammoniacal liquor is 1: 0.2～0.6, organic dispersing agent account for the solubility magnesium salts gross weight 2～4%, temperature of reaction is 40～50 ℃, stirring velocity is 300～400rpm, and the reaction times is 60min at least, obtains throw out magnesium hydroxide presoma; Described organic dispersing agent is one or more mixing in oxalic acid, trolamine, citric acid, EDTA, ethylene glycol, glycerol and the polyoxyethylene glycol;
(2) the magnesium hydroxide presoma is calcined 1～3h under 500～600 ℃ of conditions, obtain flake nano magnesium oxide.
2. a kind of preparation method of flaky nano-sized magnesium oxide according to claim 1 is characterized in that described solubility magnesium salts is sal epsom, magnesium nitrate or magnesium chloride.
3. a kind of preparation method of flaky nano-sized magnesium oxide according to claim 1 is characterized in that the magnesian outward appearance of described flake nano is a sheet, and thickness is at 13～36nm.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724734A (en) * | 2013-12-18 | 2015-06-24 | 中国科学院福建物质结构研究所 | Method for producing flower-like sphere type nanometer magnesium hydroxide with characteristics of light weight and high specific surface area |
| CN105668596A (en) * | 2016-01-05 | 2016-06-15 | 武汉工程大学 | Method for preparing plate-like basic magnesium carbonate by template induction/homogeneous precipitation |
| CN106082287A (en) * | 2016-06-14 | 2016-11-09 | 中山大学 | A kind of preparation method of magnesium oxide |
| CN106430261A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Method for preparing particle-evenly-dispersed nanometer magnesium oxide |
| CN107551990A (en) * | 2017-09-27 | 2018-01-09 | 重庆三峡学院 | A kind of preparation of magnesium hydroxide adsorbent for Dye Adsorption and its adsorption method |
| CN110203950A (en) * | 2019-06-14 | 2019-09-06 | 河北镁神科技股份有限公司 | Coating grade lithium magnesium silicate and its dedicated superfine sheet magnesia and preparation method |
| CN110436501A (en) * | 2019-08-08 | 2019-11-12 | 福州琪宁精细化工有限公司 | A kind of preparation method controlling tabular alumina size and thickness |
| CN111346594A (en) * | 2018-12-24 | 2020-06-30 | 浙江英能环保有限公司 | Preparation method of magnesium oxide nano particle cluster for adsorbing heavy metal |
| CN111450256A (en) * | 2020-04-17 | 2020-07-28 | 上海市第四人民医院 | Mesoporous magnesium hydroxide drug carrier material and preparation method and application thereof |
| CN114277614A (en) * | 2022-01-04 | 2022-04-05 | 吉林大学 | Oxide material with plasmon resonance performance and antibacterial packaging 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 |
| CN115353130A (en) * | 2022-08-26 | 2022-11-18 | 广西博世科环保科技股份有限公司 | Preparation method of defluorination nano magnesium oxide |
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| CN1865139A (en) * | 2005-05-21 | 2006-11-22 | 中国科学技术大学 | Slice type nonporous nano magnesia and its preparation method |
| CN101172626A (en) * | 2006-10-31 | 2008-05-07 | 中南大学 | Method for producing petal shaped nano-magnesia by using rhomb spar |
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| CN1865139A (en) * | 2005-05-21 | 2006-11-22 | 中国科学技术大学 | Slice type nonporous nano magnesia and its preparation method |
| CN101172626A (en) * | 2006-10-31 | 2008-05-07 | 中南大学 | Method for producing petal shaped nano-magnesia by using rhomb spar |
Non-Patent Citations (1)
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| 《人工晶体学报》 20071231 王维等 PEG对沉淀法制备纳米MgO形貌的影响 文章2.2，3.2部分，图2 1-3 第36卷, 第6期 2 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724734B (en) * | 2013-12-18 | 2017-08-25 | 中国科学院福建物质结构研究所 | A kind of manufacture lightweight, high-specific surface area, the method for bouquet type nano-sized magnesium hydroxide |
| CN104724734A (en) * | 2013-12-18 | 2015-06-24 | 中国科学院福建物质结构研究所 | Method for producing flower-like sphere type nanometer magnesium hydroxide with characteristics of light weight and high specific surface area |
| CN105668596A (en) * | 2016-01-05 | 2016-06-15 | 武汉工程大学 | Method for preparing plate-like basic magnesium carbonate by template induction/homogeneous precipitation |
| CN106082287A (en) * | 2016-06-14 | 2016-11-09 | 中山大学 | A kind of preparation method of magnesium oxide |
| CN106430261A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Method for preparing particle-evenly-dispersed nanometer magnesium oxide |
| CN107551990B (en) * | 2017-09-27 | 2020-06-09 | 重庆三峡学院 | Preparation of magnesium hydroxide adsorbent for dye adsorption and adsorption method thereof |
| CN107551990A (en) * | 2017-09-27 | 2018-01-09 | 重庆三峡学院 | A kind of preparation of magnesium hydroxide adsorbent for Dye Adsorption and its adsorption method |
| CN111346594A (en) * | 2018-12-24 | 2020-06-30 | 浙江英能环保有限公司 | Preparation method of magnesium oxide nano particle cluster for adsorbing heavy metal |
| CN110203950A (en) * | 2019-06-14 | 2019-09-06 | 河北镁神科技股份有限公司 | Coating grade lithium magnesium silicate and its dedicated superfine sheet magnesia and preparation method |
| CN110436501A (en) * | 2019-08-08 | 2019-11-12 | 福州琪宁精细化工有限公司 | A kind of preparation method controlling tabular alumina size and thickness |
| CN111450256A (en) * | 2020-04-17 | 2020-07-28 | 上海市第四人民医院 | Mesoporous magnesium hydroxide drug carrier material and preparation method and application thereof |
| CN111450256B (en) * | 2020-04-17 | 2023-10-27 | 上海市第四人民医院 | Mesoporous magnesium hydroxide drug carrier material and preparation method and application thereof |
| CN114277614A (en) * | 2022-01-04 | 2022-04-05 | 吉林大学 | Oxide material with plasmon resonance performance and antibacterial packaging application |
| CN115353130A (en) * | 2022-08-26 | 2022-11-18 | 广西博世科环保科技股份有限公司 | Preparation method of defluorination nano magnesium oxide |
| 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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Open date: 20101222 |