CN106006687A - Flower-ball-like LDHs (laminar double-metal hydroxides) and application thereof - Google Patents
Flower-ball-like LDHs (laminar double-metal hydroxides) and application thereof Download PDFInfo
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- CN106006687A CN106006687A CN201610330423.9A CN201610330423A CN106006687A CN 106006687 A CN106006687 A CN 106006687A CN 201610330423 A CN201610330423 A CN 201610330423A CN 106006687 A CN106006687 A CN 106006687A
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- 229910000000 metal hydroxide Inorganic materials 0.000 title abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 47
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 11
- 229910021645 metal ion Inorganic materials 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910052729 chemical element Inorganic materials 0.000 claims description 2
- 238000000975 co-precipitation Methods 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 230000002209 hydrophobic effect Effects 0.000 abstract description 14
- 238000001694 spray drying Methods 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 241000446313 Lamella Species 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 238000010422 painting Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000008199 coating composition Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 241000372132 Hydrometridae Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004441 surface measurement Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- 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
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
- C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Paints Or Removers (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention belongs to the technical field of preparation of inorganic materials and relates to flower-ball-like LDHs (laminar double-metal hydroxides), a preparation method and an application. Firstly, LDH slices are prepared through a T-type r Y-type microchannel reactor, the LDH slices and a surfactant are subjected to a reaction, finally, the reacted LDH slices are subjected to surface modification through spray drying, and LDHs are modified to form flower-ball-like LDHs formed by the LDH slices and having a hydrophobic property. A preparation process is simple, the repeatability is good, the cost is low, the production is environment-friendly, and the market prospect is broad; besides, by means of the unique flower-ball-like structure, flower-ball-like LDHs have an excellent hydrophobic property, and the waterproofness of a coating can be improved particularly after flower-ball-like LDHs are added to the coating.
Description
Technical field:
The invention belongs to technical field of preparation for inorganic material, relate to a kind of bouquet layered double hydroxide, preparation method and use
On the way, make duplex metal hydroxide nanometer sheet and surfactant be self-assembled into by spray drying and there is the bouquet stratiform of hydrophobic performance
Double-metal hydroxide, flower ball-shaped layered double hydroxide can improve coating property as the filler in coating.
Background technology:
Layered double hydroxide (also known as houghite, be called for short LDHs) is an anionoid type layer structure functional material,
Its chemical composition formula is: [M2+ 1-x M3+ x(OH)2]x+(An-)x/n·yH2O, wherein M2+、M3+It is in two on laminate respectively
Valency, trivalent metal ion, An-Represent interlayer anion, this kind of material due to the crystal structure of its uniqueness and physicochemical characteristic make its
Ion exchanges, adsorbs, is catalyzed, many fields such as optical material, electricity material show the most wide application prospect.Especially
It is that layered double hydroxide has good hydrophobic surface, as filler, existing water-repellent paint can be modified,
Prepare environmentally friendly coating.In Patent No. CN10104194A patent, applicant uses situ synthesis techniques, on surface
On aluminium flake after anodic oxidation, the laminated double-metal hydroxide film of synthesis has Nano/micron composite construction, at long-chain fat
After acid salt surfactant solution carries out surface hydrophobicity process, there is superior hydrophobic performance, but uncomfortable for large size plate
Close.In Patent No. ZL201210556607.9 patent, the layered double hydroxide that applicant utilizes microreactor to prepare sinks
It is coated on matrix, after shallow lake thing and hard soap self assembly, the film obtaining that there is hydrophobic performance, but the film prepared by the method is resistance to
Mill property is poor, easily comes off from matrix；Owing to LDH pattern is lamellar, improve the hydrophobicity effect of coating after drying as filler
Inconspicuous.Therefore, seek to design the double gold of hydrophobic stratiform that a kind of preparation method is simple, can significantly improve coating as filler
Belong to hydroxide very promising, and the LDHs that preparation has flower ball-shaped is a kind of effective ways solving existing issue.Wang
It is prepared for spherical MgAl-CO etc. utilizing spray drying method3LDHs, (Ind.Eng.Chem.Res.2008,47,5746-5750),
The distribution of the LDH sheet on gained ball surface is than comparatively dense, and lamellar spacing is about 50-100nm, but its hydrophobic effect is poor.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, seek a kind of bouquet and there is the double gold of stratiform of hydrophobic performance
Belong to hydroxide hybrid and preparation method thereof, solve existing lamellar layered double hydroxide and wear no resistance as coating, hold
Easily come off from matrix, and existing spherical MgAl-CO3LDHs surface lamella is the thickest, the problem of hydrophobic effect difference.
To achieve these goals, bouquet layered double hydroxide of the present invention, utilize surfactant and spray dried
The dry layered double hydroxide sheet preparing T-shaped or Y shape micro passage reaction carries out surface and modifies preparation, layered bi-metal
Hydroxide chemical formula is [M2+ 1-x M3+ x(OH)2]x+(An-)x/n·yH2O, 0.17≤x≤0.35,0≤y≤2, wherein M2+For bivalence
Metal ions M g2+、Co2+、Ni2+、Fe2+、Mn2+Or Zn2+Any one of；M3+For Al3+Or Fe3+；An-For NO3 -、
F-、Br-、Cl-、CO3 2-Or SO4 2-Any one of, the layered double hydroxide sheet at interval is stood in surface formation
Layered double hydroxide bouquet, bouquet diameter dimension is 5-10 μm, and layered double hydroxide sheet thickness is 10 ± 2nm,
Having significantly bending, in petal-shaped, contact angle is at 90-145 °, and bouquet layered double hydroxide prepares coating as filler.
The step of preparation process of bouquet layered double hydroxide of the present invention is:
(1) by soluble divalent metal salt M2+ n An- 2With soluble trivalent metal salt M2+ n An- 3Mix with deionized water and be made into
Bimetallic ion salt solution, wherein M2+For bivalent metal ion Mg2+、Co2+、Ni2+、Fe2+、Mn2+Or Zn2+In appoint
What is a kind of；M3+For Al3+Or Fe3+；An-For NO3 -、F-、Br-、Cl-、CO3 2-Or SO4 2-Any one of, configure matter
Amount mark is weak ammonia or the sodium hydroxide solution of 0.1-0.5mol/l of 3%-7%；
(2) bimetallic ion salt solution and weak ammonia or sodium hydroxide solution are joined micro passage reaction, be sufficiently mixed generation
Coprecipitation reaction obtains layered double hydroxide precipitate [M2+ 1-x M3+ x(OH)2]x+(An-)x/n·yH2O, 0.17≤x≤0.35,
0≤y≤2；
(3) layered double hydroxide precipitate deionized water prepared by step (2) is fully washed, be then dispersed in
In the surfactant solution of 0.001-0.2mol/l, react 0.1-48 hour at a temperature of 25-80 DEG C, obtain dispersion liquid；Wherein,
The chemical formula of surfactant is Cn-1H2n-1XOO-M+, n=11-22, X represent chemical element C, S, P, M+Represent monovalence
Metal ion K+、Na+；
(4) solid content by the dispersion liquid of regulation and control step (2) gained that adds water is 10-30g/L, after being spray-dried at 190 DEG C
To product bouquet layered double hydroxide.
The present invention compared with prior art, has obtained the bouquet laminated type bimetal hydroxide that surface roughness is higher, hydrophobic performance is good
Thing, has the most superior hydrophobic performance, and its preparation technology is simple, reproducible, low cost, and production environment is friendly, has
Wide market prospect；Additionally, the LDH bouquet that the LDH lamella with hydrophobic performance is built into, LDH sheet is stood at ball table
Face, the LDH lamella on surface is made up of monolayer or few layer class shepardite, has a certain distance, formed coarse between the lamella of surface
Surface, unique flower ball-shaped structure makes it be more beneficial for when preparing coating as filler playing its hydrophobic performance, the coating of preparation
There is good hydrophobicity and adhesiveness, environmental friendliness.
Accompanying drawing illustrates:
Fig. 1 is the SEM photograph that the bouquet layered double hydroxide that the embodiment of the present invention 1 relates to amplifies 3K times.
Fig. 2 is the SEM photograph that the bouquet layered double hydroxide that the embodiment of the present invention 1 relates to amplifies 30K times.
Fig. 3 is the SEM photograph that the bouquet layered double hydroxide that the embodiment of the present invention 1 relates to amplifies 50K times.
Detailed description of the invention:
Below by embodiment and combine accompanying drawing the invention will be further described.
Embodiment 1:
The bouquet layered double hydroxide preparation method that the present embodiment relates to, concrete technology step is:
(1), by Zn (NO3)2With Al (NO3)3Being dissolved in 50ml deionized water and being configured to metal ion total concentration is 0.1mol/l
Mixing salt solution, preparation 50ml concentration be the sodium hydroxide solution of 0.1mol/l；
(2), utilize micro passage reaction to make mixing salt solution and sodium hydroxide solution be sufficiently mixed and react and obtain layered bi-metal
Hydroxide (LDHs) precipitate, micro passage reaction is T-shaped, and reaction temperature is 30 DEG C；
(3), layered double hydroxide (LDHs) the precipitate deionized water prepared fully is washed, then disperse
In the potassium laurate solution that 20ml concentration is 0.1mol/l, react 2 hours at 30 DEG C；
(4) after, being spray-dried at 190 DEG C product.
Using Japan JEOL JSM-6700F field emission scanning electron microscope (SEM) to observe its surface pattern, Fig. 1-3 is to implement
The SEM figure of example 1 gained bouquet layered double hydroxide, as seen from the figure, product is that 5-10 μm is spherical, the LDH on surface
Sheet is stood on the surface of ball, in petal-shaped (Fig. 2), its Fig. 2 chooses local and amplifies further it is clear that LDH
Sheet has significantly curling, and the size estimation of sheet is about 500nm, and lamellar spacing is 10nm ± 2nm (Fig. 3), between lamella
There is obvious distance, constitute coarse surface.JC2000CD contact angle instrument LDHs hydrophobic to gained surface is used to be coated with
Layer and the contact angle of water measure, as the measured value of last contact angle after averaging after same sample surface measurement five times,
After the product tabletting of embodiment 1 preparation, surveyed contact angle is 142 ± 3 °.
It is that 11% bouquet layered double hydroxide embodiment 1 prepared adds conventional painting to as filler according to mass fraction
In material, the hydrophobicity of coating improves 36% (detailed process is shown in embodiment 5).
Embodiment 2:
The bouquet layered double hydroxide preparation method that the present embodiment relates to, concrete technology step is:
(1), by MgCO3With Al (NO3)3Being dissolved in 50ml deionized water and being configured to metal ion total concentration is 0.3mol/l
Mixing salt solution；Preparation 50ml concentration is the sodium hydroxide solution of 0.3mol/l；
(2), utilize micro passage reaction to make mixing salt solution and sodium hydroxide solution be sufficiently mixed and react and obtain layered bi-metal
Hydroxide (LDHs) precipitate, micro passage reaction is T-shaped, and reaction temperature is room temperature；
(3), layered double hydroxide (LDHs) the precipitate deionized water prepared fully is washed, then disperse
At the sodium laurate (C that 20ml concentration is 0.1mol/l11H21COONa), in solution, react 0.5 hour at 30 DEG C；
(4) after, being spray-dried at 190 DEG C product.
After product tabletting prepared by the present embodiment, surveyed contact angle is 96 ± 3 °.
It is that 10% bouquet layered double hydroxide embodiment 2 prepared adds conventional painting to as filler according to mass fraction
In material, the hydrophobicity of coating improves 15%.
Embodiment 3:
The flower ball-shaped layer double-metal hydroxide preparation method that the present embodiment relates to, concrete technology step is:
(1), by Ni (NO3)2And FeCl3Being dissolved in 50ml deionized water and being configured to metal ion total concentration is 0.1mol/l's
Mixing salt solution；Preparation 50ml concentration is the sodium hydroxide solution of 0.1mol/l；
(2), utilize micro passage reaction to make mixing salt solution and sodium hydroxide solution be sufficiently mixed and react and obtain layered bi-metal
Hydroxide (LDHs) precipitate, micro passage reaction is T-shaped, and reaction temperature is 40 DEG C；
(3), layered double hydroxide (LDHs) the precipitate deionized water prepared fully is washed, then disperse
In the potassium laurate solution that 20ml concentration is 0.001mol/l；React 0.1 hour at 80 DEG C；
(4) after, being spray-dried at 190 DEG C product.
After product tabletting prepared by the present embodiment, surveyed contact angle is 102 ± 2 °.
It is that 20% bouquet layered double hydroxide embodiment 3 prepared adds conventional painting to as filler according to mass fraction
In material, the hydrophobicity of coating improves 40%.
Embodiment 4:
The bouquet layered double hydroxide preparation method that the present embodiment relates to, concrete technology step is:
(1), by Ni (NO3)2And FeCl3Being dissolved in 50ml deionized water and being configured to metal ion total concentration is 0.1mol/l's
Mixing salt solution；The weak ammonia of preparation 50ml 7%；
(2), utilize micro passage reaction to make mixing salt solution and sodium hydroxide solution be sufficiently mixed and react and obtain layered bi-metal
Hydroxide (LDHs) precipitate, micro passage reaction is Y shape, and reaction temperature is 40 DEG C；
(3), layered double hydroxide (LDHs) the precipitate deionized water prepared fully is washed, then disperse
It is the C of 0.2mol/l in 20ml concentration12H23In SOOK solution, react 48 hours at 25 DEG C；
(4) after, being spray-dried at 190 DEG C product.
After product tabletting prepared by the present embodiment, surveyed contact angle is 92 ± 2 °.
It is that 15% bouquet layered double hydroxide embodiment 4 prepared adds conventional painting to as filler according to mass fraction
In material, the hydrophobicity of coating improves 20%.
Embodiment 5:
The preparation method of the bouquet layered double hydroxide coating that the present embodiment relates to, concrete technology step is:
Weigh epoxy resin 40 grams, organic siliconresin 10 grams, titanium dioxide 20 grams, add in agitator tank, use high speed dispersion
Machine disperses 1h under the conditions of 1000rpm, is then added in tapered mill by gained mixing paint vehicle, is ground to granularity less than 10 μm；
Weigh defoamer 0.2g, levelling agent 0.2g, the bouquet layered double hydroxide 10 grams of embodiment 1 preparation, add after grinding
Paint vehicle in, utilize high speed dispersor high speed dispersion 20min at 1500 rpm, obtain coating composition A；Weigh polyamide 50
Gram and 50 grams of acetone, high speed dispersion 1h at 1500 rpm, obtain coating composition B.One is weighed in the ratio of A:B=8:1
Determine component A and component B of quality, stir, spray on surface treated iron plate, drying at room temperature 12h, do for 60 DEG C
Dry 12h, obtains coated film sample, and measuring contact angle is 126 ± 2 °, and the hydrophobicity of coating improves 36%.
Claims (2)
1. a bouquet layered double hydroxide, it is characterised in that utilize surfactant and be spray-dried T-shaped or Y
Layered double hydroxide sheet prepared by shape micro passage reaction carries out surface and modifies preparation, layered double hydroxide chemistry
Formula is [M2+ 1-x M3+ x(OH)2]x+(An-)x/n·yH2O, 0.17≤x≤0.35,0≤y≤2, wherein M2+For bivalent metal ion Mg2+、
Co2+、Ni2+、Fe2+、Mn2+Or Zn2+Any one of；M3+For Al3+Or Fe3+；An-For NO3 -、F-、Br-、Cl-、
CO3 2-Or SO4 2-Any one of, the layered double hydroxide sheet at interval is stood at the layered bi-metal hydrogen of surface formation
Oxide bouquet, bouquet diameter dimension is 5-10 μm, and layered double hydroxide sheet thickness is 10 ± 2nm, has the most curved
Song, in petal-shaped, contact angle is at 90-145 °, and bouquet layered double hydroxide prepares coating as filler.
2. the preparation method of the bouquet layered double hydroxide described in a claim 1, it is characterised in that preparation technology walks
Suddenly it is:
(1) by soluble divalent metal salt M2+ n An- 2With soluble trivalent metal salt M2+ n An- 3Mix with deionized water and be made into
Bimetallic ion salt solution, wherein M2+For bivalent metal ion Mg2+、Co2+、Ni2+、Fe2+、Mn2+Or Zn2+In appoint
What is a kind of；M3+For Al3+Or Fe3+；An-For NO3 -、F-、Br-、Cl-、CO3 2-Or SO4 2-Any one of, configure matter
Amount mark is weak ammonia or the sodium hydroxide solution of 0.1-0.5mol/l of 3%-7%；
(2) bimetallic ion salt solution and weak ammonia or sodium hydroxide solution are joined micro passage reaction, be sufficiently mixed generation
Coprecipitation reaction obtains layered double hydroxide precipitate [M2+ 1-x M3+ x(OH)2]x+(An-)x/n·yH2O, 0.17≤x≤0.35,
0≤y≤2；
(3) layered double hydroxide precipitate deionized water prepared by step (2) is fully washed, be then dispersed in
In the surfactant solution of 0.001-0.2mol/l, react 0.1-48 hour at a temperature of 25-80 DEG C, obtain dispersion liquid；Wherein,
The chemical formula of surfactant is Cn-1H2n-1XOO-M+, n=11-22, X represent chemical element C, S, P, M+Represent monovalence
Metal ion K+、Na+；
(4) solid content by the dispersion liquid of regulation and control step (2) gained that adds water is 10-30g/L, after being spray-dried at 190 DEG C
To product bouquet layered double hydroxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610330423.9A CN106006687B (en) | 2016-05-18 | 2016-05-18 | A kind of bouquet layered double hydroxide and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610330423.9A CN106006687B (en) | 2016-05-18 | 2016-05-18 | A kind of bouquet layered double hydroxide and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740115A (en) * | 2017-11-06 | 2018-02-27 | 桂林奥尼斯特节能环保科技有限责任公司 | A kind of novel magnesium alloy sacrificial anode |
| CN110182833A (en) * | 2019-06-03 | 2019-08-30 | 肇庆学院 | It is a kind of to be crosslinked the preparation method of houghite, water paint and preparation method thereof |
| CN110564188A (en) * | 2019-09-11 | 2019-12-13 | 亚士漆(上海)有限公司 | Sand-in-water coating and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544355A (en) * | 2009-05-05 | 2009-09-30 | 北京化工大学 | Method for preparing layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis |
| CN105460899A (en) * | 2015-11-23 | 2016-04-06 | 桂林理工大学 | Preparation method of high-concentration exfoliation-type layered double hydroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544355A (en) * | 2009-05-05 | 2009-09-30 | 北京化工大学 | Method for preparing layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis |
| CN105460899A (en) * | 2015-11-23 | 2016-04-06 | 桂林理工大学 | Preparation method of high-concentration exfoliation-type layered double hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| YAYUE SUN ET AL: ""Hydrothermal Synthesis of Modified Hydrophobic Zn–Al-layered Double Hydroxides Using Structure-Directing Agents and Their Enhanced Adsorption Capacity for p-Nitrophenol"", 《ADSORPTION SCIENCE & TECHNOLOGY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740115A (en) * | 2017-11-06 | 2018-02-27 | 桂林奥尼斯特节能环保科技有限责任公司 | A kind of novel magnesium alloy sacrificial anode |
| CN110182833A (en) * | 2019-06-03 | 2019-08-30 | 肇庆学院 | It is a kind of to be crosslinked the preparation method of houghite, water paint and preparation method thereof |
| CN110182833B (en) * | 2019-06-03 | 2021-06-15 | 肇庆学院 | Preparation method of cross-linked hydrotalcite-like compound, water-based paint and preparation method thereof |
| CN110564188A (en) * | 2019-09-11 | 2019-12-13 | 亚士漆(上海)有限公司 | Sand-in-water coating and preparation method and application thereof |
| CN110564188B (en) * | 2019-09-11 | 2021-07-30 | 亚士漆(上海)有限公司 | Sand-in-water coating and preparation method and application thereof |
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| CN106006687B (en) | 2017-07-28 |
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