CN1359853A - Acidular or flaky nano magnesium hydroxide and its preparing process - Google Patents
Acidular or flaky nano magnesium hydroxide and its preparing process Download PDFInfo
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- CN1359853A CN1359853A CN 00135436 CN00135436A CN1359853A CN 1359853 A CN1359853 A CN 1359853A CN 00135436 CN00135436 CN 00135436 CN 00135436 A CN00135436 A CN 00135436A CN 1359853 A CN1359853 A CN 1359853A
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Abstract
A process for preparing acicular or flaky nano magnesium hydroxide cystal used as additive of flame retarding agent or for preparing nano magnesium oxide includes such steps as adding surfactant to the aqueous solution containing Mg ions, stirring, adding alkali solution dropwise at 10-60 deg.C, and precipitation. Its advantages are simple process, low cost and continuous production.
Description
The present invention relates to nano-sized magnesium hydroxide and preparation method thereof technical field.
Since the nineties, nano material receives great concern.Compare with bulk material, nano material has excellent mechanics, electricity, optics, magnetic property and reactive behavior.Regrettably, because existing preparation method of nano material more complicated is difficult to carry out scale operation so far.Recently, Germany " advanced material " magazine (AdvancedMaterials, 2000,12, No.11, the 818-821 page or leaf) reported that high-purity magnesium powder and distilled water with 99.999% are raw material, are solvent with the 1, under 180 ℃, high pressure, kept 20 hours, prepared bar-shaped nano-sized magnesium hydroxide.But this method reaction yield is lower, cost is higher.In addition, do not see other nano crystals magnesium hydroxide and preparation method's report as yet.
The present invention proposes a kind of needle-like or flake nano level magnesium hydroxide crystal and preparation method thereof.
Needle-like of the present invention or flake nano-magnesium hydrate crystalline preparation method is characterized in that: add tensio-active agent in containing the aqueous solution of magnesium ion, after stirring, drip alkaline solution at 10-60 ℃ and carry out precipitin reaction; Throw out gets the white powder product through distilled water wash, filtration, drying, grinding.
The described aqueous solution that contains magnesium ion comprises the aqueous solution of magnesium chloride, magnesium nitrate or sal epsom, and its concentration is 5～40% (wt);
Described tensio-active agent can be anion surfactant sodium oleate or potassium oleate, also can be the compound of nonionogenic tenside OP-10 and sodium oleate or potassium oleate; Total consumption of tensio-active agent is the 0.5-3% (wt) of magnesium ion aqueous solution total amount;
It is the sodium hydroxide of 2-15% (wt) or the aqueous solution of potassium hydroxide that described alkaline solution can adopt concentration, or the ammoniacal liquor of 10-30% (wt).
Nanometric magnesium hydroxide of the present invention is characterised in that it is needle-like or laminar magnesium hydroxide crystal; Its needle-like crystal is of a size of 3-6nm at short-axis direction, long axis direction is of a size of 50-100nm; Its laminar crystalline is long or wide all in the 150nm scope, and thickness is at 3-10nm.
Powdery product of the present invention is scattered in the ethanol, behind the ultra-sonic dispersion, observes under TEM, as seen it is needle-like or laminar crystal; Needle-like crystal is of a size of 3-6nm at short-axis direction, and long axis direction is of a size of 50-100nm; Laminar crystal is long and wide all in the 150nm scope, and thickness is between 3-10nm; For the product that obtains under the identical conditions, its size distribution is even.
Compare with bulk material, magnesium hydroxide powder of the present invention is along with the reduction of nano particle diameter, and its fluorescent emission ability and raman spectrum strength increase substantially, and have shown tangible quantum size effect.The thermal weight loss test shows that also the rate-of-loss of coolant of nanometric magnesium hydroxide improves greatly.
Product of the present invention can be used as the additive of low cigarette, Halogen, nontoxic flame-retardant polymer, because its particle diameter is a nano level, can increase substantially its oxygen index and flame retardant effect under identical magnesium hydroxide consumption; In addition, the polymer materials that contains nanometric magnesium hydroxide is the masterpiece time spent outside, and its stress spaced point is much more, and the toughness of material improves, and intensity increases.
Nanometric magnesium hydroxide product of the present invention is owing to there is very large specific surface, the reactive behavior height, and the acid waste or be used for atmosphere desulfurization, heavy metal desulfurization of can be used for neutralizing can reduce the quantity discharged of pollutent more effectively.
Nanometric magnesium hydroxide product of the present invention also can be used to produce nano level magnesium oxide, as the raw material of high-performance ceramic, electronic product and support of the catalyst.
The preparation method of the present invention nano-sized magnesium hydroxide method bar-shaped with having preparation now compared, owing to adopt the synthesis under normal pressure under the lesser temps, production technique is simple.Simultaneously, the raw material that is adopted is an inorganic magnesium salt cheap and easy to get, material concentration very high (40%) during the synthesis nano magnesium hydroxide, thereby nanometric magnesium hydroxide is produced in serialization in enormous quantities.In addition, the nanometric magnesium hydroxide of the present invention preparation since surface adsorption tensio-active agent, can prevent nanometric magnesium hydroxide powder normal agglomeration that takes place in storage, processing and use.
Accompanying drawing 1-6 is respectively transmission electron microscope (TEM) photo of embodiment of the invention 1-6 products obtained therefrom.
Accompanying drawing 7 is the typical wide angle X-diffraction of product of the present invention (XRD) spectrograms.
Accompanying drawing 8 is the typical Fourier's infrared absorption of product of the present invention (FTIR) spectrograms.
Measure powdery product of the present invention with Rigaku D/Mar rA X-diffractometer, typical X RD diffraction spectrogram as shown in Figure 7, among the figure ordinate zou be diffraction peak intensity, X-coordinate for scanning angle (2 θ); The position of all diffraction peaks is consistent with the magnesium hydroxide of JCPDS 7-239 among Fig. 7, illustrates that product of the present invention is a magnesium hydroxide.And the obvious broadening of the diffraction peak among Fig. 7 is indicated as nanometer materials.
With magnesium hydroxide powder of the present invention KBr compressing tablet, with Nicolet MAGNA-IR 750 infrared spectrometer analyzing molecules structures, typical infrared spectrogram as shown in Figure 8.Ordinate zou is the transmitance (%) of absorption peak among the figure, and X-coordinate is wave number (cm
-1).Among Fig. 8 2916 and 2854cm
-1The absorption peak at place shows that the nanometric magnesium hydroxide powder surface has superscribed tensio-active agent, and this upper layer has stoped the reunion of nanoparticle.
Below be embodiments of the invention.
Embodiment 1:
The 20g magnesium chloride is dissolved in the 30g distilled water, add potassium oleate 0.25g, the aqueous sodium hydroxide solution that slowly drips 15% (wt) is to pH value 8.5, temperature of reaction is controlled at 20-25 ℃, after precipitin reaction finishes, place the 30min slaking, after distilled water wash, filtration, the gained paste in 70 ℃ of oven dry down, grinding, is obtained white powder.Measure the product that obtains in the present embodiment with Rigaku D/MarrA X-diffractometer, its XRD diffraction spectrogram as shown in Figure 7, among the figure ordinate zou be diffraction peak intensity, X-coordinate is the angle (2 θ) of scanning; The position of all diffraction peaks is consistent with the magnesium hydroxide of JCPDS 7-239 among Fig. 7, illustrates that product of the present invention is a magnesium hydroxide.And the obvious broadening of the diffraction peak among Fig. 7 is indicated as nanometer materials.Show that through XRD calculating this powder is being nanometric magnesium hydroxide, (001) direction is of a size of 5nm.With this powder in ethanol behind the ultra-sonic dispersion, with transmission electron microscope (TEM) direct viewing particle diameter and pattern and take pictures down.Accompanying drawing 1 is depicted as the electromicroscopic photograph that the magnesium hydroxide that obtains in the present embodiment amplifies 50,000 times.Photo shows that this product is the nano level needle-like crystal, and its short-axis direction is of a size of 5nm, is of a size of 100nm at long axis direction.The fluorescence spectrum test shows that this embodiment product is compared with the magnesium hydroxide of SILVER REAGENT, and fluorescence intensity improves 3 times.The thermal weight loss test shows that the rate-of-loss of coolant of this enforcement nanometric magnesium hydroxide improves 10%.
Embodiment 2
The 10g magnesium chloride is dissolved in the 40g distilled water, add OP-10 tensio-active agent 1.5g, slowly the aqueous sodium hydroxide solution of Dropwise 5 % (wt) is to pH value 8.5, precipitation reaction temperature is controlled at 20-25 ℃, after reaction finishes, place the 20min slaking, after distilled water wash, filtration, the gained paste in 70 ℃ of oven dry down, grinding, is obtained white powder.The position of all diffraction peaks is consistent with the magnesium hydroxide of JCPDS 7-239 in its XRD diffraction spectrogram, illustrates that product of the present invention is a magnesium hydroxide.And the obvious broadening of the diffraction peak among the figure is indicated as nanometer materials.Show that through XRD calculating this powder is a nanometric magnesium hydroxide, (001) direction is of a size of 4nm.With this powder with ethanol ultra-sonic dispersion after, with transmission electron microscope (TEM) time direct viewing particle diameter and pattern and take pictures.Accompanying drawing 2 is depicted as the electromicroscopic photograph that the magnesium hydroxide that obtains in the present embodiment amplifies 50,000 times.Photo shows that this product is the nano level needle-like crystal, and its short-axis direction is of a size of 4nm, is of a size of 80nm at long axis direction.With magnesium hydroxide powder of the present invention KBr compressing tablet, with Nicolet MAGNA-IR 750 infrared spectrometer analyzing molecules structures, its infrared spectrogram as shown in Figure 8, ordinate zou is the transmitance (%) of absorption peak among the figure, X-coordinate is wave number (cm
-1).2916cm in the IR spectrum shown in Figure 8
-1And 2854cm
-1The absorption peak at place shows that the powder surface of nanometric magnesium hydroxide of the present invention has superscribed amorphous surfactant materials, and this upper layer has stoped the cohesion of ultramicron.The thermal weight loss test shows that the rate-of-loss of coolant of this enforcement nanometric magnesium hydroxide improves 20%.The Raman spectrum test shows, compares with the magnesium hydroxide of SILVER REAGENT, and raman scattering intensity improves 8 times.
Embodiment 3
The 20g magnesium chloride is dissolved in the 30g distilled water, add potassium oleate 0.5g and OP-10 tensio-active agent 1.0g, temperature is controlled at 10-12 ℃, the aqueous sodium hydroxide solution that slowly drips 15% (wt) is to pH value 8.5, after precipitin reaction finishes, after distilled water wash, filtration, the gained paste in 70 ℃ of oven dry down, grinding, is obtained white powder.The XRD analysis of powder shows that this product is a nanometric magnesium hydroxide, and (001) direction is of a size of 3nm.With this powder with ethanol ultra-sonic dispersion after, at transmission electron microscope (TEM) direct viewing particle diameter and pattern and take pictures down.Accompanying drawing 3 is depicted as the electromicroscopic photograph that the magnesium hydroxide that obtains in the present embodiment amplifies 50,000 times.Photo shows that this product is the nano level needle-like crystal, and its short-axis direction is of a size of 3nm, is of a size of 50nm at long axis direction.The size distribution of powder is very even.The fluorescence spectrum test shows that this embodiment product is compared with the magnesium hydroxide of SILVER REAGENT, and fluorescence intensity improves 8 times.2916cm shown in its infrared spectra
-1And 2854cm
-1The absorption peak at place shows that the powder surface of this nanometric magnesium hydroxide has superscribed amorphous tensio-active agent, and this upper layer has stoped the cohesion of nanoparticle.The Raman spectrum test shows, compares with the magnesium hydroxide of SILVER REAGENT, and raman scattering intensity improves 12 times.
Embodiment 4
The 20g magnesium nitrate is dissolved in the 30g distilled water, add potassium oleate 0.5g and OP-10 1.0g, temperature is controlled at 6-8 ℃, the potassium hydroxide aqueous solution that slowly drips 8% (wt) is to pH value 8.5, after precipitin reaction finishes, after distilled water wash, filtration, the gained paste in 70 ℃ of oven dry down, grinding, is obtained white powder.The position of all diffraction peaks is consistent with the magnesium hydroxide of JCPDS 7-239 in its XRD diffraction spectrogram, illustrates that product of the present invention is a magnesium hydroxide.And the obvious broadening of the diffraction peak among the figure is indicated as nanometer materials.With this powder with ethanol ultra-sonic dispersion after, at transmission electron microscope (TEM) direct viewing particle diameter and pattern and take pictures down.Accompanying drawing 4 amplifies 50,000 times electromicroscopic photograph for the magnesium hydroxide that obtains in the present embodiment.Photo shows that this product is the laminar crystal of nano level, and it is long and wide all in the 30nm scope, and thickness is approximately 3nm.The fluorescence spectrum test shows that this embodiment product is compared with the magnesium hydroxide of SILVER REAGENT, and fluorescence intensity improves 6 times.Shown in the infrared spectrogram 2916 and 2854cm
-1The absorption peak at place shows that the nanometric magnesium hydroxide powder surface has superscribed tensio-active agent, and this upper layer has stoped the cohesion of nanoparticle.The Raman spectrum test shows, compares with the magnesium hydroxide of SILVER REAGENT, and raman scattering intensity improves 16 times.The XRD of powder and IR analysis revealed, this product are nanometric magnesium hydroxide, and (001) direction is of a size of 3nm.
Embodiment 5
The 20g magnesium nitrate is dissolved in the 30g distilled water, add potassium oleate 0.15g, temperature be controlled at slowly drip 12% (wt) about 50 ℃ potassium hydroxide aqueous solution to pH value 8.5, after precipitin reaction finishes, place slaking in 60 minutes, with distilled water wash once, after the filtration, the gained paste in 70 ℃ of oven dry down, grinding, is obtained white powder.With this powder with ethanol ultra-sonic dispersion after, at transmission electron microscope (TEM) direct viewing particle diameter and pattern and take pictures down.Accompanying drawing 5 is depicted as the electromicroscopic photograph that the magnesium hydroxide that obtains in the present embodiment amplifies 20,000 times.Photo shows that this product is the laminar crystal of nano level, and it is long and wide all in the 150nm scope, and thickness is approximately 10nm.The XRD of powder and IR analysis revealed, this product are nanometric magnesium hydroxide, and (001) direction is of a size of 10nm.
Embodiment 6
The 20g magnesium chloride is dissolved in the 30g distilled water, add sodium oleate 1.0g, the aqueous sodium hydroxide solution that slowly drips 15% (wt) is to pH value 8.5, precipitation reaction temperature is controlled at 20-25 ℃, after reaction finishes, places slaking in 40 minutes, with distilled water wash once, after the filtration, the gained paste in 70 ℃ of oven dry down, grinding, is obtained white powder.With this powder with ethanol ultra-sonic dispersion after, at transmission electron microscope (TEM) direct viewing particle diameter and pattern and take pictures down.Accompanying drawing 6 is depicted as the electromicroscopic photograph that the magnesium hydroxide that obtains in the present embodiment amplifies 50,000 times.Photo shows this product for being the nano level needle-like crystal, and its short-axis direction is of a size of 4nm, is of a size of 90nm at long axis direction.The XRD of powder and IR analysis revealed, this product are nanometric magnesium hydroxide, and (001) direction is of a size of 4nm.
Claims (5)
1, a kind of needle-like or flake nano-magnesium hydrate crystalline preparation method is characterized in that: add tensio-active agent in containing the aqueous solution of magnesium ion, after stirring, drip alkaline solution at 10-60 ℃ and carry out precipitin reaction; Throw out gets the white powder product through distilled water wash, filtration, drying, grinding.
2, needle-like as claimed in claim 1 or flake nano-magnesium hydrate crystalline preparation method are characterised in that the described aqueous solution that contains magnesium ion comprises the aqueous solution of magnesium chloride, magnesium nitrate or sal epsom, and its concentration is 5～40% (wt).
3, needle-like as claimed in claim 1 or flake nano-magnesium hydrate crystalline preparation method, being characterised in that described tensio-active agent can be anion surfactant sodium oleate or potassium oleate, also can be the compound of nonionogenic tenside OP-10 and sodium oleate or potassium oleate; Total consumption of tensio-active agent is the 0.5-3% (wt) of magnesium ion aqueous solution total amount.
4, needle-like as claimed in claim 1 or flake nano-magnesium hydrate crystalline preparation method are characterised in that it is the sodium hydroxide of 2-15% (wt) or the aqueous solution of potassium hydroxide that described alkaline solution adopts concentration, or the ammoniacal liquor of 10-30% (wt).
5, a kind of nanometric magnesium hydroxide is characterised in that it is needle-like or laminar magnesium hydroxide crystal; Its needle-like crystal is of a size of 3-6nm at short-axis direction, long axis direction is of a size of 50-100nm; Its laminar crystalline is long or wide all in the 150nm scope, and thickness is at 3-10nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295270C (en) * | 2005-02-23 | 2007-01-17 | 杨第伦 | Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom |
| CN100357394C (en) * | 2006-05-29 | 2007-12-26 | 太原理工大学 | Preparation method of hydrophobic ultrafine nanometer fire retardant magnesium hydroxide |
| WO2008041833A1 (en) | 2006-10-03 | 2008-04-10 | Servicios Industriales Peñoles, S.A. De C.V. | Method for producing stable, monodispersed, nanometric magnesium hydroxide and resulting product |
| CN100422084C (en) * | 2005-05-21 | 2008-10-01 | 中国科学技术大学 | Slice type nonporous nano magnesia and its preparation method |
| CN100465247C (en) * | 2007-01-31 | 2009-03-04 | 中北大学 | Method of preparing high-purity high-dispersion magnesium hydroxide fire retardant |
| CN101054190B (en) * | 2007-04-25 | 2010-05-19 | 中国日用化学工业研究院 | Method of preparing surface modified nano magnesium hydroxide |
| CN101847467A (en) * | 2010-04-28 | 2010-09-29 | 常州市新东方电缆有限公司 | Manufacture method of ultrathin compound thin-wall insulated cable for high-speed trains |
| CN101935058A (en) * | 2010-09-17 | 2011-01-05 | 西南科技大学 | Preparation method of magnesium hydroxide hexagonal crystal |
| CN101481829B (en) * | 2009-01-20 | 2012-06-06 | 浙江依莱特纺织有限公司 | Coloured flame-retardant polypropylene fibre, preparation and use thereof |
| CN103849924A (en) * | 2014-02-12 | 2014-06-11 | 沈阳理工大学 | Method for preparing nano-magnesium hydroxide whisker by using magnesium hydroxide whisker |
| CN104109448A (en) * | 2014-07-21 | 2014-10-22 | 天津金海兴业科技有限公司 | Novel nanometer magnesium hydroxide flame retardant coating |
| CN104528779A (en) * | 2014-12-10 | 2015-04-22 | 石河子大学 | Preparation method of nano magnesium hydroxide material |
| CN105926002A (en) * | 2016-05-20 | 2016-09-07 | 西北师范大学 | Method for preparing sheet-shaped nanometer Mg(OH)2 by using electrolyte diaphragm discharge plasma |
| CN110078101A (en) * | 2019-05-30 | 2019-08-02 | 福建农林大学 | A kind of preparation and application of anti-tealeaves fungal disease nano-sized magnesium hydroxide |
| CN110359317A (en) * | 2019-07-03 | 2019-10-22 | 复旦大学 | A kind of thin layer Nanometer hydroxide multifunctional protective agent and its preparation method and application |
| CN110980780A (en) * | 2019-12-21 | 2020-04-10 | 聊城大学 | Preparation method of flaky magnesium hydroxide flame retardant |
| CN114318367A (en) * | 2022-01-10 | 2022-04-12 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
| CN114470300A (en) * | 2022-03-28 | 2022-05-13 | 浙江蓝禾医疗用品有限公司 | Fluorescent nano dressing and preparation method thereof |
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2000
- 2000-12-19 CN CN 00135436 patent/CN1359853A/en active Pending
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295270C (en) * | 2005-02-23 | 2007-01-17 | 杨第伦 | Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom |
| CN100422084C (en) * | 2005-05-21 | 2008-10-01 | 中国科学技术大学 | Slice type nonporous nano magnesia and its preparation method |
| CN100357394C (en) * | 2006-05-29 | 2007-12-26 | 太原理工大学 | Preparation method of hydrophobic ultrafine nanometer fire retardant magnesium hydroxide |
| US20110045299A1 (en) * | 2006-10-03 | 2011-02-24 | Servicios Industriales Penoles ,S.A. De C.V. | Method for producing stable, monodispersed, nanometric magnesium hydroxide and resulting product |
| WO2008041833A1 (en) | 2006-10-03 | 2008-04-10 | Servicios Industriales Peñoles, S.A. De C.V. | Method for producing stable, monodispersed, nanometric magnesium hydroxide and resulting product |
| CN100465247C (en) * | 2007-01-31 | 2009-03-04 | 中北大学 | Method of preparing high-purity high-dispersion magnesium hydroxide fire retardant |
| CN101054190B (en) * | 2007-04-25 | 2010-05-19 | 中国日用化学工业研究院 | Method of preparing surface modified nano magnesium hydroxide |
| CN101481829B (en) * | 2009-01-20 | 2012-06-06 | 浙江依莱特纺织有限公司 | Coloured flame-retardant polypropylene fibre, preparation and use thereof |
| CN101847467A (en) * | 2010-04-28 | 2010-09-29 | 常州市新东方电缆有限公司 | Manufacture method of ultrathin compound thin-wall insulated cable for high-speed trains |
| CN101935058B (en) * | 2010-09-17 | 2012-05-23 | 西南科技大学 | Preparation method of magnesium hydroxide hexagonal crystal |
| CN101935058A (en) * | 2010-09-17 | 2011-01-05 | 西南科技大学 | Preparation method of magnesium hydroxide hexagonal crystal |
| CN103849924A (en) * | 2014-02-12 | 2014-06-11 | 沈阳理工大学 | Method for preparing nano-magnesium hydroxide whisker by using magnesium hydroxide whisker |
| CN103849924B (en) * | 2014-02-12 | 2016-06-29 | 沈阳理工大学 | A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker |
| CN104109448A (en) * | 2014-07-21 | 2014-10-22 | 天津金海兴业科技有限公司 | Novel nanometer magnesium hydroxide flame retardant coating |
| CN104528779A (en) * | 2014-12-10 | 2015-04-22 | 石河子大学 | Preparation method of nano magnesium hydroxide material |
| CN105926002A (en) * | 2016-05-20 | 2016-09-07 | 西北师范大学 | Method for preparing sheet-shaped nanometer Mg(OH)2 by using electrolyte diaphragm discharge plasma |
| CN110078101A (en) * | 2019-05-30 | 2019-08-02 | 福建农林大学 | A kind of preparation and application of anti-tealeaves fungal disease nano-sized magnesium hydroxide |
| CN110078101B (en) * | 2019-05-30 | 2022-02-01 | 福建农林大学 | Preparation and application of tea fungus disease resistant nano magnesium hydroxide |
| CN110359317A (en) * | 2019-07-03 | 2019-10-22 | 复旦大学 | A kind of thin layer Nanometer hydroxide multifunctional protective agent and its preparation method and application |
| CN110980780A (en) * | 2019-12-21 | 2020-04-10 | 聊城大学 | Preparation method of flaky magnesium hydroxide flame retardant |
| CN110980780B (en) * | 2019-12-21 | 2022-06-07 | 聊城大学 | Preparation method of flaky magnesium hydroxide flame retardant |
| CN114318367A (en) * | 2022-01-10 | 2022-04-12 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
| CN114318367B (en) * | 2022-01-10 | 2023-10-27 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
| CN114470300A (en) * | 2022-03-28 | 2022-05-13 | 浙江蓝禾医疗用品有限公司 | Fluorescent nano dressing and preparation method thereof |
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