CN107858747A - A kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film - Google Patents
A kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film Download PDFInfo
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- CN107858747A CN107858747A CN201710662513.2A CN201710662513A CN107858747A CN 107858747 A CN107858747 A CN 107858747A CN 201710662513 A CN201710662513 A CN 201710662513A CN 107858747 A CN107858747 A CN 107858747A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
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Abstract
A kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film, belongs to technical field of preparation for inorganic material.The present invention is using activated magnesia as raw material, magnesia is configured to the suspension of certain initial solids content with distilled water, chemical additives are added into magnesia magma, under hydrothermal conditions, after reacting 0.5 5h, filter, wash, drying, being evenly distributed, the hydroxide nanoparticle film of the high grade of transparency.Mild condition of the present invention, technique are simple, energy-conserving and environment-protective, and product can be grown on the surface of different matrix material.The hydroxide nanoparticle film prepared using the present invention is evenly distributed, transparency is high, can be applied to produce the industrial circles such as solar cell, composite membrane, high-performance inorganic molecular screen membrane, flame-retardant additive, food preservative, magnetic material processing, heavy metal removing agent.
Description
Technical field
The present invention relates to a kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film, belongs to inorganic material and prepares skill
Art field.
Background technology
Magnesium hydroxide film has filling, fire-retardant and Tobacco Control triple capabilities, can make inorganic additive flame retardant, or prepare
The important presoma of nano oxidized magnesium film.Its specific surface area is big, activity is high, has very strong adsorption capacity, can be used as in soda acid
With agent, fume desulfurizing agent, heavy metal removing agent, the Ni to be damaged to environment is adsorbed and removed from different industrial wastes2+、
Co2+、Cr3+Etc. heavy metal ion.
Magnesium hydroxide film not only possesses above-mentioned traditional industrial use, can also be applied to high-technology field.Hydrogen-oxygen
Change magnesium film to can be used for manufacturing dye-sensitized cell, it coats TiO2The core shell structure of formation, battery conversion efficiency can be improved.
It also has high resistivity and high transmittance, is adapted to the cushion for doing CIGS solar cell in theory, but also can be by adding
Enter some metals or it is nonmetallic reduce band gap width, and then improve its electric conductivity, requiring high transmittance and high conductivity
There are certain potentiality in transparent conductive material field.In addition, in order to which the advantage of two kinds of different materials is combined, and reduce it as far as possible
Drawback, magnesium hydroxide can combine to form composite membrane with other materials.Wherein, there is polymer film easy to operate, energy consumption to reduce
It has been applied etc. advantage in business.Meanwhile the high-performance inorganic prepared using other materials such as zeolite and magnesium hydroxides
Molecular screen membrane is also developed, and the cost of these inorganic film process is lower than polymer film.
Because magnesium ion and hydroxyl rapid crystallization nucleation in the solution, and stable nucleus does not have the time slowly to grow,
Even if therefore preparing flake magnesium hydroxide is also required to ageing and hydro-thermal process for a long time, and magnesium hydroxide film is more difficult to make
It is standby.At present, the preparation method of magnesium hydroxide film mainly includes electrochemical deposition method and chemical precipitation method.Lv Ying etc. is with SnO2Lead
Electric glass is negative electrode, and permanent potential deposition is carried out to 0.1mol/L magnesium nitrate aqueous solutions system, is prepared in obvious (011) face preferentially
The magnesium hydroxide film of orientation, but the rise of deposition potential or initial pH value can cause the increase of magnesium hydroxide secondary nucleation amount, make
Obtain the uniformity and bad stability of magnesium hydroxide film.Happy and auspicious Zou Guang dragons of Chen Wei etc. make additive with ionic liquid, pass through electricity
The aqueous solution of solution magnesium nitrate makes the magnesium hydroxide film that microscopic appearance is nano flower-like, but the ionic liquid added can also trigger
Secondary nucleation, single nano flake can aggregation formation flower-like crystallite, and sedimentation potential and sedimentation time are all without making flower-like structure
Disappear.Ching-Fei Li etc. carry out negative electrode deposition reaction in magnesium nitrate solution, and flake magnesium hydroxide meeting dense accumulation is in Pt
Surface, but thin slice is not an entirety, easily separated to each other to come off, the stability of coating film has much room for improvement.Electrochemistry is sunk
Area method controls nucleation and the growth of crystal by controlling potential, and then controls the growth of magnesium hydroxide film, can rapidly prepare
Go out film product, but the electric conductivity and uniformity of required matrix and membrane material are difficult to be guaranteed, solution may be to being formed
Film have some pollutions etc., and electrolytic deposition process generally requires the facility of costliness and higher energy operates, thus cost compared with
Height, and certain difficulty be present in terms of membrane structure is controlled.
Therefore hydroxide nanoparticle film is prepared by chemical precipitation method, sedimentation at present mainly using magnesium chloride and ammoniacal liquor as
Raw material, slow down settling rate using gas diffusion method to prepare hydroxide nanoparticle film.Inghui Mao and hair will equality
Magnesium hydroxide crystal seed is prepared with magnesium chloride solution and ammoniacal liquor reaction, organic fiber surface of the crystal after modification occurs two
Secondary growth, more uniform sheet-like magnesium hydroxide crystal film is made, but needed the time up to 14 days or so.Although sedimentation
Investment it is low, it is low to prepare cost, energy-conserving and environment-protective, but the reaction time is long.And when the reaction time is longer, product pattern is easily by two
Dimension compact structure becomes three-dimensional flower-shaped structure, therefore also limits its industrialized production significantly.
How using low cost chemical precipitation method, prepare within a short period of time be uniformly distributed, the hydrogen of high transmittance
Characterization of nano-magnesium oxide thin Film is technical barrier to be resolved.During being grown in magnesium hydroxide crystal, crystal nucleation and
Crystal growth be difficult control, therefore control magnesium hydroxide nucleation rate, be magnesium hydroxide crystal can be grown into it is main because
One of element.Therefore in the growth course of film, it is magnesium hydroxide along one-dimensional long key of looking unfamiliar that can stably provide magnesium source.And
The reaction rate of magnesium salts and alkali is difficult to control, and therefore, the activity of the invention by controlling magnesia, controls the growth of magnesium hydroxide
Speed.Meanwhile in order to avoid secondary nucleation, crystallize the destruction brought to the uniformity and stability of film, use specific crystalline substance
Type derivant induces magnesium hydroxide edge（001）Crystal face grows.In order to promote magnesium hydroxide crystal to be grown along one-dimensional face is stable,
Using hydro-thermal process, crystallization and growth of the control magnesium hydroxide nucleus on other crystal faces of magnesium hydroxide and Yang Hua fans surface so that
One-dimensional face oriented growth of the magnesium hydroxide primitive of magnesia dissolving generation along magnesium hydroxide, it is thin to prepare hydroxide nanoparticle
Film.
The content of the invention
For deficiency of the prior art, prepare magnesium hydroxide it is an object of the invention to provide a kind of magnesia hydro-thermal and receive
The method of rice film, this method mild condition, technique are simple, energy-conserving and environment-protective, and product can be grown on the surface of different matrix material.Profit
Be evenly distributed with the hydroxide nanoparticle film for preparing of the present invention, transparency is high, can be applied to produce solar cell, composite membrane,
The industrial circles such as high-performance inorganic molecular screen membrane, flame-retardant additive, food preservative, magnetic material processing, heavy metal removing agent.
In order to realize foregoing invention target, the technical solution adopted by the present invention is.
A kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film, it is characterised in that methods described includes following step
Suddenly.
The first step, magnesia is configured to the suspension that initial solids content is 0.05-3 wt% with distilled water.
Second step, chemical additives are added into suspension, and chemical additives are ethylene glycol, monoethanolamine, diethanol amine
With the one or more in triethanolamine, the addition of chemical additives is 0.01-10 wt%.
3rd step, the suspension for adding chemical additives being subjected to hydro-thermal process, hydrothermal temperature is 120 DEG C ~ 250 DEG C,
The hydro-thermal time is the h of 0.5 h ~ 5, and mixing speed is 100 ~ 1500 r/min.
4th step, after hydro-thermal reaction terminates, suction filtration, ethanol washing, 95 DEG C of low temperature dryings, it is evenly distributed, high transparency
The individual layer hydroxide nanoparticle film of degree.
Step（1）Described in magnesia be using magnesite, shepardite, bischofite, dolomite or salt lake bittern as original
Material, the activated magnesia obtained after cleaning, calcining, the Δ n that activated magnesia is measured with chlorion absorption methodCl -More than 5
mol/kg。
Compared with Technical comparing, the present invention has advantage following prominent：（1）The present invention utilizes the oxidation with suitable active
Magnesium realizes the control to magnesium hydroxide growth rate, produces that the source resource of this kind of magnesia is extensive, and cost is cheap.
（2）The present invention develops the crystal formation derivant for preparing magnesium hydroxide film, and the type medicament can make magnesium hydroxide brilliant
Body success self assembly generation single thin film, its application substantially reduce the production cycle, reduce the production cost of product.
（3）Compared with existing magnesium hydroxide film technology of preparing, the present invention can quickly prepare uniform, stable hydrogen-oxygen
Change magnesium film, there is the advantages such as the simple, energy-conserving and environment-protective of mild condition, technique, a wide range of industrialized production can be achieved, have wide
Development prospect.
Brief description of the drawings
Fig. 1 is that the SEM of the final products magnesium hydroxide of embodiment 1 schemes.
Fig. 2 is the XRD of the final products magnesium hydroxide of embodiment 1.
Fig. 3 is that the SEM of the final products magnesium hydroxide of embodiment 2 schemes.
Fig. 4 is the XRD of the final products magnesium hydroxide of embodiment 2.
Fig. 5 is that the SEM of the final products magnesium hydroxide of embodiment 3 schemes.
Fig. 6 is the XRD of the final products magnesium hydroxide of embodiment 3.
Embodiment
Embodiment 1：
Take Δ nCl -It is put into 1500 ml distilled water for the 5 mol/kg g of activated magnesia 20 and is configured to magnesium hydroxide suspension
Liquid, then toward the ethylene glycol amine solution that 12 ml concentration are 100 wt% is added in magnesia magma, be put into autoclave and enter water-filling
Thermal response, hydrothermal temperature are 140 DEG C, and the hydro-thermal time is 3 h, and mixing speed is 300 r/min, after hydro-thermal reaction terminates, is taken out
Filter, washing, filter, dry 3 h at last 95 DEG C, be evenly distributed, the individual layer hydroxide nanoparticle film of the high grade of transparency.
SEM photograph and the XRD spectrum difference of product are as depicted in figs. 1 and 2.
Embodiment 2：
Take Δ nCl -It is put into 1500 ml distilled water for the 12 mol/kg g of activated magnesia 20 and is configured to magnesium hydroxide suspension
Liquid, then toward the diethanolamine solution that 10 ml concentration are 100 wt% is added in magnesia magma, be put into autoclave and enter water-filling
Thermal response, hydrothermal temperature are 180 DEG C, and the hydro-thermal time is 2 h, and mixing speed is 200 r/min, after hydro-thermal reaction terminates, is taken out
Filter, washing, filter, dry 3 h at last 95 DEG C, be evenly distributed, the individual layer hydroxide nanoparticle film of the high grade of transparency.
SEM photograph and the XRD spectrum difference of product are as shown in Figure 3 and Figure 4.
Embodiment 3：
Take Δ nCl -It is put into 1500 ml distilled water for the 15 mol/kg g of activated magnesia 20 and is configured to magnesium hydroxide suspension
Liquid, then toward the triethanolamine solution that 15 ml concentration are 100 wt% is added in magnesia magma, be put into autoclave and enter water-filling
Thermal response, hydrothermal temperature are 200 DEG C, and the hydro-thermal time is 1.5 h, and mixing speed is 150 r/min, after hydro-thermal reaction terminates,
Filter, washing, filtering, dry 3 h at last 95 DEG C, be evenly distributed, the individual layer hydroxide nanoparticle of the high grade of transparency is thin
Film.SEM photograph and the XRD spectrum difference of product are as shown in Figure 5 and Figure 6.
Claims (2)
1. a kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film, it is characterised in that methods described includes following step
Suddenly：
（1）The first step, magnesia is configured to the suspension that initial solids content is 0.05-3 wt% with distilled water；
（2）Second step, crystal formation control is added into suspension, and chemical additives are ethylene glycol, monoethanolamine, diethanol amine and three
One or more in monoethanolamine, the addition of chemical additives is 0.01-10 wt%；
（3）3rd step, the suspension for adding crystal formation control is subjected to hydro-thermal process, hydrothermal temperature is 120 DEG C ~ 250 DEG C, hydro-thermal
Time is the h of 0.5 h ~ 5, and mixing speed is 100 ~ 1500 r/min；
（4）4th step, after hydro-thermal reaction terminates, suction filtration, ethanol washing, 95 DEG C of low temperature dryings, it is evenly distributed, the high grade of transparency
Individual layer hydroxide nanoparticle film.
2. the method that a kind of magnesia hydro-thermal according to claim 1 prepares hydroxide nanoparticle film, it is characterised in that：
Step（1）Described in magnesia be using magnesite, shepardite, bischofite, dolomite or salt lake bittern as raw material, through except
The activated magnesia obtained after miscellaneous, calcining, the Δ n that activated magnesia is measured with chlorion absorption methodCl -More than 5 mol/kg.
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| CN201710662513.2A CN107858747B (en) | 2017-08-04 | 2017-08-04 | Method for preparing magnesium hydroxide nano film by magnesium oxide hydrothermal method |
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| CN201710662513.2A CN107858747B (en) | 2017-08-04 | 2017-08-04 | Method for preparing magnesium hydroxide nano film by magnesium oxide hydrothermal method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269827A (en) * | 2008-04-02 | 2008-09-24 | 浙江工业大学 | Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method |
| CN102259898A (en) * | 2011-06-30 | 2011-11-30 | 武汉钢铁(集团)公司 | Method for preparing magnesium hydroxide utilizing light-burned dolomite powder |
| CN102491380A (en) * | 2011-12-06 | 2012-06-13 | 中国科学院过程工程研究所 | Method for preparing flaky magnesium hydroxide |
-
2017
- 2017-08-04 CN CN201710662513.2A patent/CN107858747B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269827A (en) * | 2008-04-02 | 2008-09-24 | 浙江工业大学 | Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method |
| CN102259898A (en) * | 2011-06-30 | 2011-11-30 | 武汉钢铁(集团)公司 | Method for preparing magnesium hydroxide utilizing light-burned dolomite powder |
| CN102491380A (en) * | 2011-12-06 | 2012-06-13 | 中国科学院过程工程研究所 | Method for preparing flaky magnesium hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| YONGBIN CHEN, ET AL.: "A novel preparation of nanosized hexagonal Mg(OH)2 as a flame retardant", 《PARTICUOLOGY》 * |
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