CN107673378B - A kind of method that magnesia hydration prepares hydroxide nanoparticle film - Google Patents
A kind of method that magnesia hydration prepares hydroxide nanoparticle film Download PDFInfo
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- CN107673378B CN107673378B CN201710662514.7A CN201710662514A CN107673378B CN 107673378 B CN107673378 B CN 107673378B CN 201710662514 A CN201710662514 A CN 201710662514A CN 107673378 B CN107673378 B CN 107673378B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
A kind of method that magnesia hydration prepares hydroxide nanoparticle film, belongs to technical field of preparation for inorganic material.The present invention is using activated magnesia as raw material, organic solvent is added and is made into magnesia organic suspension liquid, magnesia magma is added in distilled water and carries out aquation, chemical additives are added in hydration process, after aquation 0.5-3h, it filters, washing, drying, is evenly distributed, the single layer nanometric magnesium hydroxide film of the high grade of transparency.Mild condition of the present invention, simple process, energy conservation and environmental protection, product can be grown on the surface of different matrix material.Prepared by the method nanometric magnesium hydroxide film is evenly distributed, transparency is high, can be applied to the industrial circles such as production 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 methods that magnesia hydration prepares hydroxide nanoparticle film, belong to inorganic material preparation skill
Art field.
Background technique
Magnesium hydroxide film has filling, fire-retardant and tobacco control triple capabilities, can make inorganic additive flame retardant, or preparation
The important presoma of nano oxidized magnesium film.Its large specific surface area, activity are high, have very strong adsorption capacity, can be used as in soda acid
With agent, fume desulfurizing agent, heavy metal removing agent, is adsorbed from different industrial wastes and remove the Ni to cause damages to environment2+、
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
Changing magnesium film can be used for manufacturing dye-sensitized cell, it coats TiO2The core-shell structure of formation can improve battery conversion efficiency.
It also has high resistivity and high transmittance, is theoretically suitble to do the buffer layer of CIGS solar cell, but can also 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 combine the advantage of two kinds of different materials, and reduce it to the greatest extent
Drawback, magnesium hydroxide can combine with other materials and form composite membrane.Wherein, there is polymer film easy to operate, energy consumption to reduce
Etc. advantages be applied 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 of magnesium ion and hydroxyl rapid crystallization nucleation in the solution, and the nucleus generated does not have the time slowly to grow,
Even if therefore preparing general pattern such as flake magnesium hydroxide is also required to ageing and hydro-thermal process for a long time, and film-form hydroxide
Magnesium is more difficult to prepare.Currently, the preparation method of magnesium hydroxide film mainly includes electrochemical deposition method and chemical precipitation method.Lv Ying
Deng with SnO2Electro-conductive glass is cathode, carries out permanent potential deposition to 0.1mol/L magnesium nitrate aqueous solution system, prepares in obvious
(011) magnesium hydroxide film of face preferred orientation, but the raising of deposition potential or initial pH value will lead to magnesium hydroxide it is secondary at
Core amount increases, so that the uniformity and bad stability of magnesium hydroxide film.Happy and auspicious Zou Guang dragon of Chen Wei etc. makees to add with ionic liquid
Add agent, the aqueous solution by being electrolysed magnesium nitrate produces the magnesium hydroxide film that microscopic appearance is nano flower-like, but the ion added
Liquid can also cause secondary nucleation, single nano flake meeting aggregation formation flower-like crystallite, and sedimentation potential and sedimentation time are not
Flower-like structure can be made to disappear.Ching-Fei Li et al. carries out cathode deposition reaction, flake magnesium hydroxide meeting in magnesium nitrate solution
Dense accumulation is on the surface Pt, however thin slice is not an entirety, is easily separated off to each other, and the stability of coating film needs to be mentioned
It is high.Electrochemical deposition method controls the nucleation and production of crystal by control potential, and then controls the growth of magnesium hydroxide film, energy
Rapidly prepare film product, but the electric conductivity and uniformity of required matrix and membrane material are difficult to be guaranteed, solution
There may be some pollutions etc. to the film of formation, and electrolytic deposition process generally requires expensive facility and higher energy to operate,
Therefore higher cost, and there are certain difficulties in terms of controlling membrane structure.
Therefore hydroxide nanoparticle film is prepared by chemical precipitation method, the precipitation method are mainly with magnesium chloride and ammonium hydroxide at present
Raw material slows 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 ammonium hydroxide reaction, organic fiber surface of the crystal after modification occurs two
Secondary growth has produced more uniform sheet-like magnesium hydroxide crystal film, but needs the time up to 14 days or so.Although sedimentation
Investment it is low, preparation cost is low, energy conservation and environmental protection, but the reaction time is too long.And when the reaction time is longer again, product pattern easily by
Two-dimentional compact structure becomes three-dimensional flower-shaped structure, therefore also limits its industrialized production significantly.
How using low cost chemical precipitation method, within a short period of time prepare be uniformly distributed, high transmittance is received
Rice magnesium hydroxide film is technical problem to be resolved.Due to during magnesium hydroxide crystal is grown, crystal nucleation and
Crystal growth is difficult to control, thus 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, can steadily provide magnesium source be the key that magnesium hydroxide along it is one-dimensional look unfamiliar it is long.And
The reaction rate of magnesium salts and alkali is not easy to control, therefore, activity and addition manner of the present invention by control magnesia, control oxidation
The hydration rate of magnesium, and then control the growth rate of magnesium hydroxide.Meanwhile in order to avoid secondary nucleation, crystallization are to the equal of film
Even property and stability bring are destroyed, and magnesium hydroxide is induced to grow along (001) crystal face using specific crystal form inducer.In order to
Promote magnesium hydroxide crystal that can stablize along one-dimensional face to grow, and magnesium hydroxide is prevented to be nucleated in mgo surface, prevents oxidation
Magnesium aquation controls magnesium hydroxide nucleus in the crystallization and life of other crystal faces of magnesium hydroxide and mgo surface using ultrasonic treatment
It is long, so that the magnesium hydroxide primitive that magnesia dissolution generates prepares magnesium hydroxide along the one-dimensional face oriented growth of magnesium hydroxide
Nano thin-film.
Summary of the invention
Aiming at the shortcomings in the prior art, magnesium hydroxide is prepared the purpose of the present invention is to provide a kind of magnesia hydration to receive
The method of rice film, this method mild condition, simple process, energy conservation and environmental protection, product can be grown on the surface of different matrix material.Benefit
It is evenly distributed with nanometric magnesium hydroxide film prepared by the present invention, transparency is high, can be applied to production solar cell, compound
The industry neck such as film, high-performance inorganic molecular screen membrane, flame-retardant additive, food preservative, magnetic material processing, heavy metal removing agent
Domain.
In order to realize that foregoing invention target, the technical solution adopted by the present invention be.
A kind of method that magnesia hydration prepares hydroxide nanoparticle film, it is characterised in that the method includes walking as follows
Suddenly.
(1) make organic solvent with one or both of ethyl alcohol, isopropanol, it is 5- that magnesia, which is made into solid content,
The solution of 30wt%, then magnesia organic suspension liquid is made in ultrasonic disperse 1-30min.
(2) magnesia organic suspension liquid is added in distilled water with certain rate of addition and carries out hydration reaction, magnesia
Organic suspension liquid adds completion in 10min, and in the preceding 20min of hydration reaction, crystal form control is added with certain rate of addition
Preparation solution, chemical additives are one of ethylene glycol, monoethanolamine, diethanol amine and triethanolamine or a variety of, and aquation is anti-
Mechanical stirring or ultrasonic treatment should be used, when magnesia organic suspension liquid completion of dropwise addition, the initial solids content of magnesia is
0.05-3wt%, the content of chemical additives is 0.01-10wt% in solution when crystal form controls skill completion of dropwise addition.
(3) it after hydration reaction, filters, washing, drying, is evenly distributed, the single layer magnesium hydroxide of the high grade of transparency
Nano thin-film.
Magnesia as described in step (1) is with magnesite, shepardite, bischofite, dolomite or salt lake bittern for original
Material, obtained activated magnesia after being cleaned, being calcined, the Δ n measured with chloride ion absorption methodCl - 5mol/kg。
The ultrasonic frequency of ultrasonic disperse as described in step (1) is 20-40kHz, power 50-3000w.
At 50-90 DEG C, the time of hydration reaction is 0.5-3 hours for the temperature control of hydration reaction in step (2).
Mechanical stirring described in step (2) is high-shear emulsifying stirring, and stirring rate 500-5000r/min is described
Ultrasonic treatment ultrasonic frequency be 20-40kHz, power 50-3000w.
Compared with Technical comparing the invention has the following outstanding advantages: (1) heretofore described magnesia can be water chestnut
Magnesium mine, shepardite, bischofite, dolomite or salt lake bittern be raw material, cleaned, calcine after obtain activated magnesia production
The source resource of this kind of magnesia is extensive, low in cost.
(2) present invention realizes the control to magnesium hydroxide growth rate using the magnesia with suitable active, so that
The growth of magnesium hydroxide nucleus and the growth of crystal carry out simultaneously.
(3) present invention finds the crystal form inducer for preparing magnesium hydroxide film, the type medicament can make magnesium hydroxide brilliant
Body success self assembly generates single thin film, its application substantially reduces the production cycle, reduces the production cost of product.
(4) compared with existing magnesium hydroxide film technology of preparing, carrying out hydration reaction under normal pressure of the present invention can be quick
Uniform and stable magnesium hydroxide film is prepared, has the advantages such as mild condition, simple process, energy conservation and environmental protection, it can be achieved that big model
Industrialized production is enclosed, there is vast potential for future development.
Detailed description of the invention.
Fig. 1 is that the SEM of 1 final products magnesium hydroxide of embodiment schemes.
Fig. 2 is the XRD diagram of 1 final products magnesium hydroxide of embodiment.
Fig. 3 is that the SEM of 2 final products magnesium hydroxide of embodiment schemes.
Fig. 4 is the XRD diagram of 2 final products magnesium hydroxide of embodiment.
Fig. 5 is that the SEM of 3 final products magnesium hydroxide of embodiment schemes.
Fig. 6 is the XRD diagram of 3 final products magnesium hydroxide of embodiment
Specific embodiment.
Embodiment 1:
Take Δ nCl -It is put into beaker for the activated magnesia 2g of 10mol/kg, 20ml ethyl alcohol is added, is placed on the frequency of ultrasonic wave
Rate and power are set to carry out decentralized processing 10min in the supersonic wave cleaning machine of 20kHz, 50w, at 65 DEG C, preparation
Magnesia magma is added drop-wise to progress hydration reaction 1h in 150ml distilled water with the rate of 3ml/min, is starting that magnesia is added dropwise
It is added at one time the triethanolamine solution that 10ml concentration is 10wt% while suspension, carries out high shear always in hydration process
Emulsification stirring, stirring rate are set as 2000r/min, after hydration reaction, filter, washing, filtering, dry at last 105 DEG C
5h is evenly distributed, the single layer nanometric magnesium hydroxide film of the high grade of transparency.The SEM photograph and XRD spectrum of product are respectively such as
Shown in Fig. 1 and Fig. 2.
Embodiment 2:
Take Δ nCl -It is put into beaker for the activated magnesia 2g of 15mol/kg, 10ml ethyl alcohol is added, is placed on the frequency of ultrasonic wave
Rate and power are set to carry out decentralized processing 15min in the supersonic wave cleaning machine of 28kHz, 100w, at 80 DEG C, preparation
Magnesia magma is added drop-wise to progress hydration reaction 1.5h in 200ml distilled water with the rate of 2ml/min, when reacting 5min
5ml concentration is added as the ethylene glycol solution of 8wt% with the rate of 1ml/min, is ultrasonically treated always in aquation, ultrasonic wave
Frequency and power are set to 40kHz, 100w, after hydration reaction, filter, washing, filtering, dry 5h at last 105 DEG C,
It is evenly distributed, the single layer nanometric magnesium hydroxide film of the high grade of transparency.The SEM photograph and XRD spectrum of product are respectively such as Fig. 3
With shown in Fig. 4.
Embodiment 3:
Take Δ nCl -It is put into beaker for the activated magnesia 2g of 25mol/kg, 10ml isopropanol is added, is placed on ultrasonic wave
Frequency and power are set to carry out decentralized processing 10min in the supersonic wave cleaning machine of 40kHz, 50w, at 75 DEG C, preparation
Magnesia magma progress hydration reaction 2h is added drop-wise in 200ml distilled water with the rate of 1ml/min, in reaction 10min
When the monoethanolamine solution that 8ml concentration is 10wt% is added with the rate of 3ml/min, carry out high-shear emulsifying always in aquation and stir
It mixes, stirring rate is set as 3000r/min, after hydration reaction, filters, washing, filtering, dries 5h at last 105 DEG C, obtains
It is uniformly distributed, the single layer nanometric magnesium hydroxide film of the high grade of transparency.The SEM photograph and XRD spectrum of product are respectively such as Fig. 5 and figure
Shown in 6.
Claims (4)
1. a kind of method that magnesia hydration prepares hydroxide nanoparticle film, it is characterised in that the method includes walking as follows
It is rapid:
(1) make organic solvent with one or both of ethyl alcohol, isopropanol, it is 5-30wt%'s that magnesia, which is made into solid content,
Solution, then magnesia organic suspension liquid is made in ultrasonic disperse 1-30min；
(2) magnesia organic suspension liquid is added in distilled water with certain rate of addition and carries out hydration reaction, magnesia is organic
Suspension adds completion in 10min, and in the preceding 20min of hydration reaction, chemical additives are added with certain rate of addition
Solution, chemical additives are one of ethylene glycol, monoethanolamine, diethanol amine and triethanolamine or a variety of, and hydration reaction makes
With mechanical stirring or ultrasonic treatment, when magnesia organic suspension liquid completion of dropwise addition, the initial solids content of magnesia is 0.05-3
Wt%, the content of chemical additives is 0.01-10wt% in solution when crystal form controls completion of dropwise addition；
(3) it after hydration reaction, filters, washing, drying, is evenly distributed, the single layer nanoscale hydroxide of the high grade of transparency
Magnesium film；
Wherein the magnesia is activated magnesia, the Δ n that the activated magnesia is measured with chloride ion absorption methodCl -It is greater than
5mol/kg。
2. the method that a kind of magnesia hydration according to claim 1 prepares hydroxide nanoparticle film, it is characterised in that:
The ultrasonic frequency of ultrasonic disperse as described in step (1) is 20-40KHz, power 50-3000w.
3. the method that a kind of magnesia hydration according to claim 1 prepares hydroxide nanoparticle film, it is characterised in that:
At 50-90 DEG C, the time of hydration reaction is 0.5-3 hours for the temperature control of hydration reaction in step (2).
4. the method that a kind of magnesia hydration according to claim 1 prepares hydroxide nanoparticle film, it is characterised in that:
Mechanical stirring described in step (2) is that high-shear emulsifying stirs, stirring rate 500-5000r/min, at the ultrasound
The ultrasonic frequency of reason is 20-40KHz, power 50-3000w.
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| CN108950649A (en) * | 2018-07-02 | 2018-12-07 | 山东科技大学 | A kind of preparation method of magnesium/magnesium alloy surface by micro-arc oxidation water-bath sealing of hole composite coating |
| CN111763116A (en) * | 2020-07-13 | 2020-10-13 | 广西南宁华夏农业科技有限公司 | Organic-inorganic compound fertilizer capable of adjusting acid, supplementing magnesium and preventing plant yellowing and preparation method thereof |
| CN111747790A (en) * | 2020-07-13 | 2020-10-09 | 广西南宁华夏农业科技有限公司 | Organic-inorganic compound fertilizer containing magnesium hydroxide and preparation method thereof |
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| CN102659146B (en) * | 2012-04-28 | 2014-09-17 | 中国科学院福建物质结构研究所 | Method for preparing flame retardant magnesium hydroxide |
| CN102774862B (en) * | 2012-08-14 | 2014-04-16 | 河北联合大学 | Method for preparing flame-retardant magnesium hydroxide by hydration |
| WO2015051482A1 (en) * | 2013-10-11 | 2015-04-16 | 河北联合大学 | Method for manufacturing sheet monodisperse nano-magnesium hydroxide by using magnesite |
| CN103864121B (en) * | 2014-03-20 | 2015-08-19 | 大连理工大学 | A kind of high solid-liquid ratio aquation prepares the method for magnesium hydroxide |
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