CN108912739A - A kind of preparation method of super-hydrophobic amorphous metal boride Nanoalloy material - Google Patents

A kind of preparation method of super-hydrophobic amorphous metal boride Nanoalloy material Download PDF

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CN108912739A
CN108912739A CN201810775210.6A CN201810775210A CN108912739A CN 108912739 A CN108912739 A CN 108912739A CN 201810775210 A CN201810775210 A CN 201810775210A CN 108912739 A CN108912739 A CN 108912739A
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acid
metal boride
amorphous metal
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苏钽
秉琦明
刘靖尧
王志秀
董韬文
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Jilin University
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds

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Abstract

The invention discloses a kind of preparation methods of super-hydrophobic amorphous metal boride Nanoalloy material, belong to technical field of nanometer material preparation, first synthesis amorphous metal boride (MBx, M=Fe, Co, Ni；X=0.1-1.0) Nanoalloy material, the material morphology are black amorphous state stratiform fold thin layer；Secondly, synthesizing super-hydrophobic metal boride (MBx, M=Fe, Co, Ni；X=0.1-1.0) Nanoalloy material, the material are black nano particle.This method is suitable for the preparation of a variety of nano superhydrophobic amorphous alloy materials, for prepared nano material while with excellent ultra-hydrophobicity, synthesis cost is lower, and preparation method is simply easy to assembly line synthesis, adjustability is stronger according to demand, is conducive to large scale preparation and application.This method significantly reduces the use to environment and the harmful silicon fluoride class compound of biology, and product is environmentally protective, is easy to resource recycling.

Description

A kind of preparation method of super-hydrophobic amorphous metal boride Nanoalloy material
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of super-hydrophobic amorphous metal boride nanometer The preparation method of alloy material.
Background technique
There is the materials of the superhydrophobic properties such as such as lotus leaf surface in nature, and which results in the concerns of researcher. After carefully studying, it has been found that the surface of these materials is all by being similar to the micro-nano structure and low surface that Bird's Nest stacks Energy substance is constituted, and the combination of exactly the two makes its surface have super-hydrophobic property.Due to droplet connecing in super hydrophobic surface Contacting surface product is very small, it is possible to which phenomena such as effective burn into frost for inhibiting surface, chlorination, electric current conduct is a kind of good Protective materials.Further, since water droplet cannot stablize stop on super-hydrophobic surface, when inclination angle is greater than 5 °, water droplet will It tumbling without leaving any trace, while the dust and dirt on surface can be taken away, this makes the material surface have self-cleaning function, Therefore super hydrophobic surface has extremely wide application prospect.For example, it can be on ship, during reducing ship running Resistance, and promote its erosion-resisting ability.It can also be subtracted on wind power generation blade and airframe and wire surface The overlay capacity of few ice, reduces energy consumption, improves safety coefficient.Further, it is also possible to be used in building surface, prevent from polluting, be promoted Self-cleaning ability.
Super hydrophobic coating is all to be mixed with nano particle with resin at present, be added a certain amount of adhesion agent prepare it is super-hydrophobic Coating, and these coating are all one-step synthesis.The strength of coating of one-step method preparation is not generally very well, moreover, one-step method There are problems that resin solidification, hydrophobic property is caused to fail, can then make to operate after improvement increasingly complex, takes a long time.
Summary of the invention
For the above-mentioned problems in the prior art, the object of the present invention is to provide a kind of with the non-of ultra-hydrophobicity The preparation method of amorphous metal boride nano material, first synthesis amorphous metal boride (MBx, M=Fe, Co, Ni；X= 0.1-1.0) Nanoalloy material, the material morphology are black amorphous state stratiform fold thin layer；Secondly, synthesizing super-hydrophobic metal boron Compound (MBx, M=Fe, Co, Ni；X=0.1-1.0) Nanoalloy material, the material are black nano particle.Furthermore above-mentioned On the basis of, it carries out the method for the amorphous metal boride Nanoalloy material and its there are different colours after loading different carriers With the composite material of absorption property and stronger hydrophobic property.
The present invention is achieved through the following technical solutions：
A kind of preparation method of super-hydrophobic amorphous metal boride nano material, specific step is as follows：
(1), amorphous metal boride nano material is synthesized：
It takes the aqueous solution of raw material to mix with chemical reducing agent, 0.5-5h is heated at 22-50 DEG C, filtering precipitated product is used in combination Distilled water is cleaned, and is dried in 50-110 DEG C, amorphous metal boride nano material is obtained, in the product shared by metallic element Mass fraction is between 0.1-1.0；
Wherein, the raw material are selected from MCl after treatment2(M=Fe, Co, Ni) or MSO4(M=Fe, Co, Ni), The aqueous solution of raw material and the molar ratio 1.0 of chemical reducing agent:0.5-1.0:6；The chemical reducing agent is lithium borohydride, boron Sodium hydride, potassium borohydride, ammonia borane, sodium hypophosphite, Lime Hypophosphate or hypophosphorous acid.
(2), super-hydrophobic amorphous metal boride nano material is synthesized；
The amorphous metal boride that step (1) obtains is mixed with hydrophobic surface covering, in 10-100 DEG C of constant temperature 0.5-6h is stirred, standing sedimentation washs solid product with ethyl alcohol repeatedly, and product is dried, obtains MB (M=Fe, Co, Ni) and receive The super-hydrophobic amorphous metal boride of rice.
Further, the MCl described in step (1) after treatment2Or MSO4, specifically, taking quality is 1.0 × 10- 3g-1.0×106G nano load particle, being soaked in concentration at room temperature is 1.0 × 10-4mol/L-1.0×102The MCl of mol/L2Or MSO4In (M=Fe, Co, Ni) aqueous solution, 0.5-24h is stirred, stands filtering, solid product is washed with distilled water and in 60-80 It is dried at DEG C.
Further, the nano load particle is selected from molecular sieve, metal oxide, silicon, carbon, metal organic frame material Material.
Further, the partial size of the nano load particle is 10nm-500um, aperture 0.3nm-50nm.
Further, MCl described in step (1)2Or MSO4Concentration be 1.0 × 10-4mol/L-1.0×102Mol/L, institute The concentration for the chemical reducing agent stated is 1.0 × 10-4mol/L-1.0×102mol/L。
Further, hydrophobic surface covering described in step (2) is the saturated fat containing 8 to 24 carbon atoms Acid, unsaturated fatty acid or silicon fluoride containing 8 to 24 carbon atoms.
Further, the concentration of hydrophobic surface covering described in step (2) is 1.0 × 10-4mol/L-1.0× 102mol/L。
Further, the saturated fatty acid containing 8 to 24 carbon atoms is selected from caprylic acid, n-capric acid, positive 11 Alkanoic acid, dodecanoic acid, n-tridecane acid, n-teradecanoic acid, n-pentadecane acid, Palmiticacid, n-heptadecane acid, positive 18 Alkanoic acid, NSC 77136 acid, n-eicosane acid, Heneicosane acid, behenic acid, n-tricosane acid and n-tetracosane At least one of acid.
Further, the unsaturated fatty acid containing 8 to 24 carbon atoms be selected from decylenic acid, dodecenoic acid, Tetradecenoic acid, gaidic acid, hexadecadienoic acid, octadecenoic acid, octadecadienoic acid, octatecatrienoic acid, 18 Carbon tetraenoic acid, eicosenoic acid, eicosadienoic acid, eicosatrienoic acid, eicosatetraenoic acid, eicosapentaenoic acid, 20 Two carbon enoic acids, two dodecadienoic acids, docosatrienoic acid, docosatetraenoic acid, clupanodonic acid and 24 At least one of carbon enoic acid.
Further, the silicon fluoride is selected from ten trifluoro octyl trimethoxy silanes, ten trifluoro octyl triethoxysilicanes At least one of alkane, heptadecafluorodecyl triethoxysilane and 17 fluorine ruthenium trimethoxysilanes.
Compared with prior art, advantages of the present invention is as follows：
This method is suitable for the preparation of a variety of nano superhydrophobic amorphous alloy materials, and prepared nano material has While excellent ultra-hydrophobicity, synthesis cost is lower, and preparation method is simply easy to assembly line synthesis, can adjust according to demand Property it is stronger, be conducive to large scale preparation and application.In addition, being shown during preparing the nano superhydrophobic amorphous alloy material The use reduced to environment and the harmful silicon fluoride class compound of biology is write, product is environmentally protective, is easy to resource recycling.
Detailed description of the invention
Fig. 1：The transmission electron microscope photo of nano superhydrophobic amorphous state nickel borides prepared by the embodiment of the present invention 2；
Fig. 2：The scanning for the molecular sieve carried super-hydrophobic amorphous state nickel borides that under different multiples prepared by the embodiment of the present invention 4 Electromicroscopic photograph；
Wherein, a is 1000 times of amplification, b is 15000 times of amplification, and c is 30000 times of amplification, and d is 40000 times of amplification；
Fig. 3：Test the surface tension of the hydrophobic ability of nano superhydrophobic amorphous state nickel borides prepared by the embodiment of the present invention 1 Figure；
Fig. 4：Test the table of the molecular sieve carried super-hydrophobic hydrophobic ability of amorphous state nickel borides prepared by the embodiment of the present invention 4 Face tonogram.
As shown in Figure 1, from TEM transmission electron microscope photo as it can be seen that prepared nano material be in amorphous state lamelliform, have compared with Big specific surface area is conducive to prepare super hydrophobic material by surface modification.
As shown in Fig. 2, as it can be seen that (a) can be seen that nano particle is big by 1000 times of photos from SEM stereoscan photograph Small uniform, size is between the order of magnitude range of 100nm~1 μm；(b) a biggish particle in 1000 times of photos is taken to be amplified to 15000 times of observations, size is at 2 μm or so；(c) can be seen that particle surface by 30000 and 40000 times of photos with (d) is in Existing nanometer strip branched structure, the structure are conducive to improve the hydrophobic performance after material surface modification.
As shown in figure 3, the contact angle on the surface being made of nano superhydrophobic amorphous state boronation nickel material is 158.3o, explanation The material has good ultra-hydrophobicity.
As shown in figure 4, the contact angle on the surface being made of molecular sieve carried nano superhydrophobic amorphous state boronation nickel material For 156.2o, illustrate that the material has good ultra-hydrophobicity.
Specific embodiment
The present invention is described further with reference to the accompanying drawing.
Embodiment 1
The NiCl for being 0.1mol/L to 100ml concentration2In aqueous solution, the NaBH of the 1.0mol/L into 10ml is slowly added dropwise4Water Solution stirs 30min, solid product is obtained by filtration after completion of the reaction after being added dropwise, solid product is placed in 60 DEG C of normal pressure drums It is dried in wind baking oven, obtains nanometer amorphous nickel borides.
It weighs the nanometer amorphous nickel borides that 0.2g is prepared according to the above method and is scattered in ten trifluoro octyl triethoxy of 1.5ml In silane, 30min is stirred under 80 DEG C of constant temperatures, filters out solid product after completion of the reaction, washed repeatedly with dehydrated alcohol, Then solid product is dried in 60 DEG C of normal pressure convection ovens, obtains nano superhydrophobic amorphous state nickel borides.
Embodiment 2
The FeCl for being 0.5mol/L to 500ml concentration2In aqueous solution, the NaBH of the 2.0mol/L into 100ml is slowly added dropwise4 Aqueous solution stirs 60min, solid product is obtained by filtration after completion of the reaction after being added dropwise, solid product is placed in 60 DEG C of normal pressures It is dried in convection oven, obtains nanometer amorphous iron boride.
It weighs the nanometer amorphous metal iron boride that 1.0g is prepared according to the above method to mix with 5ml octadecanoid acid, at 130 DEG C Constant temperature stirs 60min, filters out solid product after completion of the reaction, is washed repeatedly with dehydrated alcohol, then by solid product 80 It is dried in DEG C normal pressure convection oven, obtains nano superhydrophobic amorphous state iron boride.
Embodiment 3
The CoCl for being 0.1mol/L to 1000ml concentration2In aqueous solution, the NaBH of the 1.5mol/L into 100ml is slowly added dropwise4 Aqueous solution stirs 60min, solid product is obtained by filtration after completion of the reaction after being added dropwise, solid product is placed in 80 DEG C of normal pressures It is dried in convection oven, obtains nanometer amorphous boronation cobalt.
Weigh the nanometer amorphous metal boronation cobalt and ten trifluoro octyl triethoxy of 20ml that 100g is prepared according to the above method Silane and the mixing of 50g octadecanoid acid stir 120min in 120 DEG C of constant temperature, solid product are filtered out after completion of the reaction, with anhydrous second Alcohol washs repeatedly, then dries solid product in 60 DEG C of normal pressure convection ovens, obtains nano superhydrophobic amorphous state boronation cobalt.
Embodiment 4
0.3g ZIF-8 powder is taken, the NiCl that 30ml concentration is 0.3mol/L is soaked under room temperature constant temperature2It is water-soluble In liquid, 60min is stirred, filtering is stood after completion of the reaction, is washed with distilled water solid product and is placed in 80 DEG C of normal pressure baking ovens and dry It is dry, obtain absorption NiCl2ZIF-8 presoma.
0.3g is adsorbed into NiCl2Nanometer ZIF-8 presoma be scattered in 100ml distilled water, at room temperature slowly The NaBH that 20ml concentration is 2.0mol/L is added dropwise4Aqueous solution, the reaction was continued 60min after being added dropwise, stood after completion of the reaction Filter solid product, and solid product is cleaned with distilled water, it is placed in 80 DEG C of normal pressure baking ovens and dries, obtain receiving for ZIF-8 load Rice amorphous state nickel borides.
The nanometer amorphous metal nickel borides that 0.2g ZIF-8 is loaded is soaked in 2ml tridecafluoro-n-octyltriethoxysilane In, 60min is stirred in 80 DEG C of constant temperature, standing sedimentation washs solid product with ethyl alcohol repeatedly, and by product in 80 DEG C of normal pressure air blast It is dried in baking oven, obtains the nano superhydrophobic amorphous state nickel borides of ZIF-8 load.
Embodiment 5
0.1-1.5g 3A molecular sieve powder is taken, the FeCl that 50ml concentration is 1mol/L is soaked under room temperature constant temperature2 In aqueous solution, 30min is stirred, filtering is stood after completion of the reaction, is washed with distilled water solid product and is placed on 50 DEG C of normal pressure baking ovens Middle drying obtains absorption FeCl2Molecular sieve precursor.
1.0g is adsorbed into FeCl23A molecular sieve precursor be dispersed in 200ml distilled water, at room temperature slowly drop Adding 50ml concentration is the NaBH of 0.5mol/L4Aqueous solution, the reaction was continued 10-60min after being added dropwise stand filtering precipitated product And cleaned with distilled water, obtain molecular sieve carried nanometer amorphous iron boride.
The molecular sieve carried nanometer amorphous metal iron boride of 0.4g is mixed with 10g octadecanoid acid, is stirred in 100 DEG C of constant temperature 10min is mixed, standing sedimentation washs solid product with ethyl alcohol repeatedly, and product is dried in 80 DEG C of normal pressure convection ovens, obtains Molecular sieve carried nano superhydrophobic amorphous state iron boride.
Embodiment 6
0.1-1.5g active carbon powder is taken, the CoCl that 100ml concentration is 2mol/L is soaked under room temperature constant temperature2Water In solution, 10min is stirred, stands filtering, stands filtering after completion of the reaction, solid product is washed with distilled water and is placed on 60 DEG C often It is dried in pressure baking oven, obtains absorption FeCl2Activated carbon precursor.
10g is adsorbed into FeCl2Activated carbon precursor be dispersed in 1000ml distilled water, be slowly added dropwise at room temperature 200ml concentration is the NaBH of 0.3mol/L4Aqueous solution, the reaction was continued 120min after being added dropwise stand filtering precipitated product simultaneously It is cleaned with distilled water, obtains activated carbon supported nanometer amorphous boronation cobalt.
By 10g activated carbon supported nanometer amorphous metal boronation cobalt and 10ml tridecafluoro-n-octyltriethoxysilane and The mixing of 30g octadecanoid acid stirs 40min in 100 DEG C of constant temperature, standing sedimentation, washs solid product repeatedly with ethyl alcohol, and by product It is dried in 80 DEG C of normal pressure convection ovens, activated carbon supported nano superhydrophobic amorphous state boronation cobalt.

Claims (9)

1. a kind of preparation method of super-hydrophobic amorphous metal boride nano material, which is characterized in that specific step is as follows：
(1), amorphous metal boride nano material is synthesized：
It takes the aqueous solution of raw material to mix with chemical reducing agent, heats 0.5-5h at 22-50 DEG C, filter precipitated product and with distilling Water is cleaned, and is dried in 50-110 DEG C, obtains amorphous metal boride nano material, quality shared by metallic element in the product Score is between 0.1-1.0；
Wherein, the raw material are selected from MCl after treatment2(M=Fe, Co, Ni) or MSO4(M=Fe, Co, Ni), former material The aqueous solution of material and the molar ratio 1.0 of chemical reducing agent:0.5-1.0:6；The chemical reducing agent is lithium borohydride, hydroboration Sodium, potassium borohydride, ammonia borane, sodium hypophosphite, Lime Hypophosphate or hypophosphorous acid；
(2), super-hydrophobic amorphous metal boride nano material is synthesized；
The amorphous metal boride that step (1) obtains is mixed with hydrophobic surface covering, is stirred in 10-100 DEG C of constant temperature 0.5-6h, standing sedimentation wash solid product with ethyl alcohol repeatedly, and product are dried, and it is super to obtain MB (M=Fe, Co, Ni) nanometer Hydrophobic amorphous metal boride.
2. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as described in claim 1, feature exist In MCl described in step (1) after treatment2Or MSO4, specifically, taking quality is 1.0 × 10-3g-1.0 × 106g nanometers Particle is loaded, being soaked in concentration at room temperature is 1.0 × 10-4mol/L-1.0 × 102mol/L MCl2Or MSO4(M=Fe, Co, Ni) in aqueous solution, 0.5-24h is stirred, stands filtering, solid product is washed with distilled water and dries at 60-80 DEG C.
3. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as claimed in claim 2, feature exist In the nano load particle is selected from molecular sieve, metal oxide, silicon, carbon, metal-organic framework material.
4. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as described in claim 1, feature exist In the concentration of MCl2 or MSO4 described in step (1) is 1.0 × 10-4mol/L-1.0 × 102mol/L, the electronation The concentration of agent is 1.0 × 10-4mol/L-1.0 × 102mol/L.
5. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as described in claim 1, feature exist In hydrophobic surface covering described in step (2) is the saturated fatty acid containing 8 to 24 carbon atoms, contains 8 to 24 carbon The unsaturated fatty acid or silicon fluoride of atom.
6. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as described in claim 1, feature exist In the concentration of hydrophobic surface covering described in step (2) is 1.0 × 10-4mol/L-1.0 × 102mol/L.
7. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as claimed in claim 5, feature exist In the saturated fatty acid containing 8 to 24 carbon atoms is selected from caprylic acid, n-capric acid, n-undecane acid, n-dodecane Acid, n-tridecane acid, n-teradecanoic acid, n-pentadecane acid, Palmiticacid, n-heptadecane acid, n-octadecane acid, NSC 77136 At least one in acid, n-eicosane acid, Heneicosane acid, behenic acid, n-tricosane acid and n-tetracosane acid Kind.
8. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as claimed in claim 5, feature exist In the unsaturated fatty acid containing 8 to 24 carbon atoms is selected from decylenic acid, dodecenoic acid, tetradecenoic acid, 16 Carbon enoic acid, hexadecadienoic acid, octadecenoic acid, octadecadienoic acid, octatecatrienoic acid, parinaric acid, 20 carbon Olefin(e) acid, eicosadienoic acid, eicosatrienoic acid, eicosatetraenoic acid, eicosapentaenoic acid, docosenoic acid, 22 At least one in carbon dienoic acid, docosatrienoic acid, docosatetraenoic acid, clupanodonic acid and tetracosenoic acid Kind.
9. a kind of preparation method of super-hydrophobic amorphous metal boride nano material as claimed in claim 5, feature exist In the silicon fluoride is selected from ten trifluoro octyl trimethoxy silanes, tridecafluoro-n-octyltriethoxysilane, 17 fluorine decyls three At least one of Ethoxysilane and 17 fluorine ruthenium trimethoxysilanes.
CN201810775210.6A 2018-07-16 2018-07-16 A kind of preparation method of super-hydrophobic amorphous metal boride Nanoalloy material Pending CN108912739A (en)

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Application publication date: 20181130