CN1242921C - Synthesis method of magnesium hydroxide nano pipe - Google Patents
Synthesis method of magnesium hydroxide nano pipe Download PDFInfo
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- CN1242921C CN1242921C CN 200410023420 CN200410023420A CN1242921C CN 1242921 C CN1242921 C CN 1242921C CN 200410023420 CN200410023420 CN 200410023420 CN 200410023420 A CN200410023420 A CN 200410023420A CN 1242921 C CN1242921 C CN 1242921C
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Abstract
The present invention provides a method for synthesizing magnesium hydroxide nanometer pipes. The method comprises the following steps: an ammonia water solution is added and stirred in a solution containing magnesium ions, and the solution is centrifugally washed into a state having neutral pH value after deposits are generated; the deposits after centrifugal washing are dispersed in the mixed solvent of methanol or ethanol and water again, and then, proper inorganic salt as a mineralizing agent is added and stirred to dissolve in the solution; the stirred and mixed mixture is moved into a closed reactor and cooled to the normal temperature after complete reactions; finally, a magnesium hydroxide nanometer pipes are obtained through washing and dryness. The solution containing magnesium ions prefers the water solution of magnesium nitrate or magnesium chloride, the mineralizing agent prefers one or the mixture of potassium chloride, sodium chloride, sodium sulfate, vulcanized kalii, potassium nitrate and sodium nitrate, the methanol or the ethanol is preferred, and the present invention has the reaction temperature of 200 to 250 DEG C and the reaction time of 15 to 24 hours.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to the production method of nano material, relate in particular to a kind of synthetic method of magnesium hydrate nanotube.
Background technology
Since carbon nanotube comes out, one-dimensional nano structure material receives much attention because of its peculiar electricity, optics, magnetic and mechanical property and the potential application in nano-device structure thereof, thereby to explore preparation low-dimension nano material structurally ordered, excellent property be the focus of relevant technologies personnel research always.Magnesium hydroxide is as a kind of common inorganics, be widely used in foodstuffs industry, smoke-discharging sulfur-removing, water treatment and other environmental protection aspect, the magnesium hydroxide of special crystalline form is a kind of, environment protecting better 2nd 1 century novel inorganic filled-type fire retardant [Wang Zheng-Zhou more superior than organic fire-retardant and ATH, et al., Plastic Science andTechnology], obtained development rapidly in countries such as the U.S., Japan, Britain in recent years, according to incompletely statistics, the annual capacity of external magnesium hydroxide has reached 1,400,000 tons.The environmental requirement of the world today is more and more higher, and research, cooperative development, the activity in production of relevant in recent years magnesium hydroxide are very active, so the demand of magnesium hydroxide can increase greatly, has bright development prospect.Because to have size little for the magnesium hydroxide nano material, specific surface area is big, strengthened and body material between interaction, can effectively improve the flame retardant effect and the mechanical property of flame retardant of magnesium hydroxide.The nineties in 20th century, the magnesium hydroxide of multiple crystalline form has been studied by countries such as U.S., day, purpose is to improve the mechanical property that improves fire retardant, just has the effect of some steel to the magnesium hydroxide nano material after for example joining in the polypropylene matrix, can substitute these steel.Especially in recent years, the relevant expert of affiliated technical field has done a lot of effort, and wherein template or tensio-active agent have obtained using widely.Yet, in reaction system, to introduce template or tensio-active agent and be unable to do without their preparation and selection, this makes that not only entire reaction course is complicated, increases preparation cost, reduces product purity, and is unfavorable for large-scale industrial production.
Summary of the invention
The purpose of this invention is to provide a kind of simple for process, cost is low, the purity height helps the synthetic method of the magnesium hydrate nanotube that large-scale industrial produces.
Purpose of the present invention can realize by following technical measures:
The synthetic method of this magnesium hydrate nanotube adopts following steps to carry out:
A, in containing the solution of magnesium ion, add ammonia soln and stir, post precipitation centrifuge washing to be generated to pH value is a neutrality; After
B, the precipitation behind centrifuge washing is dispersed in the mixed solvent of alcohol and water again, the inorganic salt of 3.5～6.9 times of weight parts that add magnesium hydroxide again are as mineralizer and stir, and make its dissolving; Then
C, will be moved into through the mixture of stirring and dissolving in the closed reactor, 200～250 ℃ of reactions 15～24 hours down, after the product through reacting completely is cooled to normal temperature; At last
D, through washing and dry, magnesium hydrate nanotube.
Purpose of the present invention also can realize by following technical measures:
The described solution that contains magnesium ion is the aqueous solution of magnesium nitrate or magnesium chloride; Described mineralizer is Repone K, sodium-chlor, sodium sulfate, potassium sulphide, saltpetre, SODIUMNITRATE or their mixture; Described alcohol is methyl alcohol or ethanol.
The present invention is a raw material with the solution that contains magnesium ion, adopt and add ammonia soln and stirring fast, magnesium hydrate precipitate to be generated, again the precipitate with deionized water of gained is repeatedly washed to the pH value be about 7, then with inorganic salt as mineralizer, reacted 15～24 hours under 200～250 ℃ of conditions in closed reactor, the product after reacting completely is cooled to normal temperature; Through washing and be drying to obtain the magnesium hydrate nanotube product.This method is not used any organic reagent of tensio-active agent or template or other, and technology is simple, and working condition is easy to control, and with low cost, the product purity height can be realized large-scale industrial production.
Embodiment
Embodiment 1:
Take by weighing the 0.001mol magnesium chloride and place beaker, add the 20ml deionized water, stirring makes its dissolving, the ammonia soln that adds 10ml 5M more rapidly, continue to stir 10 minutes, be 7 with resulting precipitation centrifuge washing to the pH value of solution then, precipitation is dispersed in the mixed solvent of 20ml first alcohol and water again, add 0.3 gram Repone K again and make its dissolving as mineralizer and stirring, to be moved into through the mixture of stirring and dissolving in the stainless steel closed reactor, reaction is 18 hours under 240 ℃ of conditions, and the postcooling that reacts completely is to normal temperature, then with resulting product deionized water wash, through 50 ℃ of dry products that get.Product is accredited as magnesium hydroxide through X-ray powder diffraction; TEM, SEM Electronic Speculum testing product pattern.
Embodiment 2:
Take by weighing the 0.001mol magnesium nitrate and place beaker, add the 20ml deionized water, stirring makes its dissolving, the ammonia soln that adds 10ml 5M more rapidly, continue to stir 10 minutes, be 7 with resulting precipitation centrifuge washing to the pH value of solution then, precipitation is dispersed in the mixed solvent of 20ml first alcohol and water again, add 0.4 gram sodium sulfate again and make its dissolving as mineralizer and stirring, to be moved into through the mixture of stirring and dissolving in the stainless steel closed reactor, reaction is 22 hours under 220 ℃ of conditions, and the postcooling that reacts completely is to normal temperature, then with resulting product deionized water wash, through 60 ℃ of dry products that get.Product is accredited as magnesium hydroxide through X-ray powder diffraction; TEM, SEM Electronic Speculum testing product pattern.
Embodiment 3:
Take by weighing the 0.001mol magnesium chloride and place beaker, add the 20ml deionized water, stirring makes its dissolving, the ammonia soln that adds 10ml 5M more rapidly, continue to stir 10 minutes, be 7 with resulting precipitation centrifuge washing to the pH value of solution then, precipitation is dispersed in the mixed solvent of 20ml first alcohol and water again, the mixture that adds 0.2 gram sodium-chlor and 0.2 gram saltpetre again makes its dissolving as mineralizer and stirring, to be moved into through the mixture of stirring and dissolving in the stainless steel closed reactor, reaction is 20 hours under 240 ℃ of conditions, and the postcooling that reacts completely is to normal temperature, then with resulting product deionized water wash, through 60 ℃ of dry products that get.Product is accredited as magnesium hydroxide through X-ray powder diffraction; TEM, SEM Electronic Speculum testing product pattern.
Embodiment 4:
Take by weighing the 0.001mol magnesium nitrate and place beaker, add the 20ml deionized water, stirring makes its dissolving, the ammonia soln that adds 10ml 5M more rapidly, continue to stir 10 minutes, be 7 with resulting precipitation centrifuge washing to the pH value of solution then, precipitation is dispersed in the mixed solvent of 20ml second alcohol and water again, add 0.2 gram potassium sulphide again and make its dissolving as mineralizer and stirring, to be moved into through the mixture of stirring and dissolving in the stainless steel closed reactor, reaction is 19 hours under 240 ℃ of conditions, and the postcooling that reacts completely is to normal temperature, then with resulting product deionized water wash, through 50 ℃ of dry products that get.Product is accredited as magnesium hydroxide through X-ray powder diffraction; TEM, SEM Electronic Speculum testing product pattern.
Description of drawings
Fig. 1 is the magnesium hydrate nanotube X-ray powder diffraction figure of the embodiment of the invention 1 preparation;
Fig. 2 is that the magnesium hydrate nanotube TEM Electronic Speculum of the embodiment of the invention 1 preparation detects the transmission photo;
Fig. 3 is that the magnesium hydrate nanotube SEM Electronic Speculum of the embodiment of the invention 1 preparation detects scanned photograph;
The magnesium hydrate nanotube TEM Electronic Speculum of Fig. 4 inventive embodiments 2 preparations detects the transmission photo.
Claims (4)
1, the synthetic method of magnesium hydrate nanotube is characterized in that this method adopts following steps to carry out:
A, in containing the solution of magnesium ion, add ammonia soln and stir, post precipitation centrifuge washing to be generated to pH value is a neutrality; After
B, the precipitation behind centrifuge washing is dispersed in the mixed solvent of alcohol and water again, the inorganic salt of 3.5～6.9 times of weight parts that add magnesium hydroxide again are as mineralizer and stir, and make its dissolving; Then
C, will be moved into through the mixture of stirring and dissolving in the closed reactor, 200～250 ℃ of reactions 15～24 hours down, after the product through reacting completely is cooled to normal temperature; At last
D, through washing and dry, magnesium hydrate nanotube.
2, the synthetic method of magnesium hydrate nanotube according to claim 1 is characterized in that the described solution that contains magnesium ion is the aqueous solution of magnesium nitrate or magnesium chloride.
3, the synthetic method of magnesium hydrate nanotube according to claim 1 is characterized in that described mineralizer is Repone K, sodium-chlor, sodium sulfate, potassium sulphide, saltpetre, SODIUMNITRATE or their mixture.
4, the method for synthetic magnesium hydrate nanotube according to claim 1 is characterized in that described alcohol is methyl alcohol or ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410023420 CN1242921C (en) | 2004-01-09 | 2004-01-09 | Synthesis method of magnesium hydroxide nano pipe |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410023420 CN1242921C (en) | 2004-01-09 | 2004-01-09 | Synthesis method of magnesium hydroxide nano pipe |
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| CN1556034A CN1556034A (en) | 2004-12-22 |
| CN1242921C true CN1242921C (en) | 2006-02-22 |
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| CN 200410023420 Expired - Fee Related CN1242921C (en) | 2004-01-09 | 2004-01-09 | Synthesis method of magnesium hydroxide nano pipe |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100425538C (en) * | 2006-10-31 | 2008-10-15 | 山东师范大学 | Synthesis method of cobaltous oxide nano-tube |
| CN100486901C (en) * | 2006-10-31 | 2009-05-13 | 山东师范大学 | Synthesis method of cobaltosic oxide nano-tube |
| CN100425539C (en) * | 2006-10-31 | 2008-10-15 | 山东师范大学 | Synthesis method of nickel hydroxide nano-tube |
| CN101555027B (en) * | 2009-05-08 | 2011-03-09 | 南京大学 | Method for preparing magnesium hydrate nanotube |
| RU2422364C9 (en) * | 2009-08-04 | 2015-11-20 | Закрытое акционерное общество "НикоМаг" | Method of producing micro- and/or nanometric magnesium hydroxide |
| CN102344153B (en) * | 2011-09-19 | 2013-01-16 | 河南科技大学 | Preparation method of nanotubular magnesium hydroxide |
| CN102674406B (en) * | 2011-12-19 | 2013-10-30 | 河南科技大学 | Preparation method of nano-tubular magnesium oxide |
| CN114655971A (en) * | 2021-12-30 | 2022-06-24 | 南京大学 | Preparation method of magnesium hydroxide nanotube |
| CN114560509A (en) * | 2021-12-30 | 2022-05-31 | 南京大学扬州化学化工研究院 | Preparation method of cobalt hydroxide and cobalt hydroxide prepared by same |
| CN115893459A (en) * | 2022-12-20 | 2023-04-04 | 山东沃特斯德新材料科技有限公司 | Preparation method of multifunctional water-soluble nano magnesium hydroxide stock solution |
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