CN105462297B - A kind of automatically cleaning water aluminum-silver slurry and preparation method thereof - Google Patents
A kind of automatically cleaning water aluminum-silver slurry and preparation method thereof Download PDFInfo
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- CN105462297B CN105462297B CN201510976658.0A CN201510976658A CN105462297B CN 105462297 B CN105462297 B CN 105462297B CN 201510976658 A CN201510976658 A CN 201510976658A CN 105462297 B CN105462297 B CN 105462297B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09C1/62—Metallic pigments or fillers
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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
- C09C1/62—Metallic pigments or fillers
- C09C1/64—Aluminium
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09C3/06—Treatment with inorganic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
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Abstract
The present invention relates to a kind of automatically cleaning water aluminum-silver slurry and preparation method thereof, the water aluminum-silver slurry is oiliness aluminum paste Surface coating TiO2Film, pass through TiO2Automatically cleaning and water solubility are realized in the photocatalysis of film, the preparation method of the water aluminum-silver slurry, first with the commercially available oiliness aluminum paste of organic solvent washing, remove the organic matter of excess surface;Secondly, oiliness aluminum paste is pre-processed using titanate coupling agent, oiliness aluminum paste surface is formed covalent key connection;Then butyl titanate is added dropwise, the titanium dioxide of tetrabutyl titanate hydrolysis is formed film on aluminum paste surface, is finally prepared into water aluminum-silver slurry.Compared with prior art, the water aluminum-silver slurry that prepared by the present invention does not influence the metallic luster of aluminium flake, has good photocatalytic self-cleaning performance.
Description
Technical field
The present invention relates to technical field of coatings, and in particular to a kind of TiO with self-cleaning function2Coating type water aluminium silver
Slurry and preparation method thereof.
Background technology
Aluminum paste is a kind of indispensable metallic pigments in production and living, is a kind of by special thin snowflake shape or silver dollar shape piece
The pulpous state aluminium pigment that alumina particles are handled through special process.Aluminum paste has good adhesive force, covering power and albedo, simultaneously
There is the effect and suspension characteristic of uniqueness, and one kind for becoming most study, being most widely used
Metallic pigments.
Along with the proposition of friendly environment society, coating also develop by gradual hydrotropismization and automatically cleaning direction.Traditional oils
Property aluminum paste is not easily dispersed in water paint, without adapting to water paint due to substantial amounts of solvent naphtha be present;Simultaneously because
Aluminium is a kind of amphoteric metal, oxidizable in meta-acid or the water paint of meta-alkali to lose metallic luster and produce hydrogen, closed
Space in can produce " rise and listen ", for production bring certain potential safety hazard.Therefore, it is necessary to the aluminium silver applied to water paint
Slurry is modified processing, to ensure the stability of water aluminum-silver slurry.
Automatic cleaning coating can make surface contaminant or dust granule automatic under the effect of the external force such as gravity, rainwater, wind-force
Come off or removed by photocatalytic degradation, there are water saving, energy-saving and environmental protection.TiO2Coating is that one kind is based on inorganic light
The automatic cleaning coating of semi-conducting material is catalyzed, its automatically cleaning principle includes two aspects:1、TiO2Produced under ultraviolet light irradiation
Raw electron-hole pair, can be with adsorbing in TiO2The H of material surface2O and O2Generation redox reaction and generate hydrogen-oxygen freedom
Base, hydroxyl free radical have very high activity, can be with decomposing organic pollutant, so as to realize self-cleaning surface;2、TiO2In light
Super parents surface can be changed into according under, makes pollutant and TiO2Intimate surface contact, photocatalysis Decomposition efficiency is improved, while also had
Pollutant is washed away beneficial to rainwater, realizes self-cleaning surface.So TiO2Material is shown well under practical service environment
Automatically cleaning characteristic, thus in automatic cleaning coating field there is the actual use bigger than super-hydrophobic coat to be worth.
The surface modifying method of aluminum paste is a lot, and classification is also different.It can substantially be divided into:Coating modification method, deposition table
Face is modified method, mechanochemical reaction, local reaction method, sol-gal process and microcapsule method etc..Coating modification method is typically in aluminium
Powder surface covers a stratification compound film, and its unique transparency will not damage the luster performance of aluminium powder, thus more be ground
Study carefully, but the compound hydrophily deficiency that prior art cladding is used, easy dry linting, and automatically cleaning can not be accomplished.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of simple to operate, production
Cost is low, does not influence the original gloss of aluminium flake, and covering power is high, the excellent automatically cleaning water aluminum-silver slurry of photocatalysis performance and its preparation side
Method.
The purpose of the present invention can be achieved through the following technical solutions:A kind of automatically cleaning water aluminum-silver slurry, it is oiliness aluminium
Silver paste Surface coating TiO2Film, pass through TiO2Automatically cleaning and water solubility are realized in the photocatalysis of film.The aluminum paste not shadow
The original gloss of aluminium flake is rung, belongs to water soluble paint, and there is good photocatalytic self-cleaning function, belongs to Environmentally friendly coatings.
A kind of preparation method of automatically cleaning water aluminum-silver slurry described above, using sol-gal process, uses organic solvent first
Commercially available oiliness aluminum paste is washed, removes the organic matter of excess surface;Secondly, oiliness aluminum paste is entered using titanate coupling agent
Row pretreatment, makes oiliness aluminum paste surface form covalent key connection;Then butyl titanate is added dropwise, makes tetrabutyl titanate hydrolysis
Titanium dioxide forms film on aluminum paste surface, is finally prepared into water aluminum-silver slurry.It specifically includes following steps:
(1) parts by weight of oiliness aluminum paste 1 are mixed with the parts by weight of acetone 1.5~3.5, removes having for oiliness aluminum paste surface
Machine thing, obtain aluminum paste solid;
(2) titanate coupling agent is mixed with organic solvent, obtains mixed solution A, by butyl titanate and organic solvent
Mixing, obtains mixed solution B;
(3) by the aluminum paste solid obtained by step (1) and the parts by weight of organic solvent 5~10, mixed solution A, the weight of water 0.1
Part is mixed, isolated solid mixture after 60~80 DEG C of reactions;
(4) solid mixture obtained by step (3) is mixed with the parts by weight of organic solvent 5~10, the parts by weight of water 0.1, adjusted
PH to 7~8, under the conditions of 60~80 DEG C, is added dropwise mixed solution B, and ageing, which separates, after reaction produces automatically cleaning water aluminum-silver slurry.
The mass ratio of the medium oil aluminum paste of step (1) and acetone is 1:(1.5~3.5).
Step (2), step (3), the organic solvent described in step (4) are alcohols solvent, including ethanol or isopropanol.
Titanate coupling agent described in step (2) includes Di(dioctylpyrophosphato) ethylene titanate and three ethanol
Chelate solution, (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three or double (the two octyloxy pyrophosphoric acid ester groups) ethylenes of amine
One kind in titanate esters.
The mass concentration of step (2) described mixed solution A is 10%;
The mass concentration of the mixed solution B is 25%-75%.
The mass ratio of aluminum paste solid and titanate coupling agent in described step (3) is 1:(0.08-0.2);It is described
The step of (4) in solid mixture and butyl titanate mass ratio be 1:(0.25-0.5).
The conditioning agent for being used to adjust pH in step (4) is triethylamine or ammoniacal liquor.
Mixed solution B time for adding is 1~5h in step (4).
Digestion time is 3~6h in step (4).
In order to characterize the performance of the automatically cleaning water aluminum-silver slurry of the present invention, field emission scanning electron microscope is utilized
(FESEM) and EDS power spectrums carry out surface topography sign and elementary analysis to the coating sample of preparation.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects:
(1) prepare simply, production cost is low.
(2) water aluminum-silver slurry Surface coating of the invention has one layer of fine and close TiO2Film, the original gold of aluminium flake is not influenceed
Belong to gloss, and due to TiO2The presence of film so that aluminum paste of the invention has good photocatalytic self-cleaning performance, is applicable
In various water-based stoving paints, water-based ink and aqueous architectural material etc..
Brief description of the drawings
Fig. 1 is the surface microscopic FESEM shape appearance figures (2 μm of ratios) of the commercially available aluminum paste of present invention acetone treatment;
Fig. 2 is the TiO that present invention gained has self-cleaning function2The surface microscopic FESEM shapes of coating type water aluminum-silver slurry
Looks figure (10 μm of ratios);
Fig. 3 is the TiO that present invention gained has self-cleaning function2The surface microscopic FESEM shapes of coating type water aluminum-silver slurry
Looks figure (2 μm of ratios);
Fig. 4 is the TiO that present invention gained has self-cleaning function2The surface microscopic EDS power spectrums of coating type water aluminum-silver slurry
Figure.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of automatically cleaning water aluminum-silver slurry, it is aluminum paste Surface coating TiO2Film, pass through TiO2The photocatalysis of film
Realize automatically cleaning and water solubility.
Above-mentioned automatically cleaning aluminum paste is prepared using sol-gal process, specifically includes following steps:
(1) the commercially available parts by weight of oiliness aluminum paste 1 are mixed with the parts by weight of acetone 1.6, isolated aluminium after certain time
Silver paste solid is stand-by;
(2) titanate coupling agent Di(dioctylpyrophosphato) ethylene titanate is mixed with isopropanol, obtains titanium
The mixed solution A of acid esters coupling agent Di(dioctylpyrophosphato) ethylene titanate volume fraction 10%;By the fourth of metatitanic acid four
Ester mixes with isopropanol, obtains the mixed solution B of butyl titanate volume fraction 25%;
(3) aluminum paste solid obtained by step (1) and the isopropanol of 9 parts by weight are taken, the mixed solution A of 1 parts by weight, and
The water of 0.1 parts by weight is mixed, and is reacted under conditions of 80 DEG C.Solid mixture separated after a period of time stand-by;
(4) solid mixture obtained by step (3) is mixed with the isopropanol of 9 parts by weight and the water of 0.1 parts by weight, uses ammonia
Water adjusts pH to 7, and the mixed solution B of 1 parts by weight is added dropwise under conditions of 60 DEG C, wherein, mixed solution B divides 2.5h uniformly to drip
Add, 4h is aged after being added dropwise to complete, then separate solid with solvent, gained solid is automatically cleaning aluminum paste.
Following performance test is carried out to the above-mentioned automatically cleaning water aluminum-silver slurry being prepared:
(1) its surface topography is observed using field emission scanning electron microscope, is to be made in the present embodiment as Figure 1-3
Automatically cleaning aluminum paste surface FESEM photos, as seen from the figure aluminum paste Surface coating have one layer of fine and close film.
(2) its surface mass, such as Fig. 4 are analyzed using field emission scanning electron microscope energy dispersive spectrometer (EDS) measure
It is shown, it is the EDS energy spectrum diagrams of obtained automatically cleaning aluminum paste in the present embodiment, surface coated one layer of aluminum paste as seen from the figure
Fine and close film is TiO2。
Embodiment 2
A kind of automatically cleaning aluminum paste preparation method, is comprised the following steps that:
(1) 1 parts by weight oiliness aluminum paste is mixed with the acetone of 2.6 parts by weight, after certain time by solid mixture with
Solvent separates;
(2) titanate coupling agent Di(dioctylpyrophosphato) ethylene titanate is mixed with isopropanol, obtains titanium
The mixed solution A of acid esters coupling agent Di(dioctylpyrophosphato) ethylene titanate mass fraction 10%;By the fourth of metatitanic acid four
Ester mixes with isopropanol, obtains the mixed solution B of butyl titanate mass fraction 25%;
(3) aluminum paste and the isopropanol of 8 parts by weight crossed acetone treatment, the mixed solution A and 0.1 weight of 1 parts by weight
The water mixing of part is measured, reacts, separates solid mixture after a period of time stand-by under conditions of 60 DEG C;
(4) solid mixture obtained by step (3) is mixed with the isopropanol of 9 parts by weight and the water of 0.1 parts by weight, uses ammonia
Water adjusts pH to 7, and the mixed solution B of 1 parts by weight is added dropwise under conditions of 60 DEG C, wherein, mixed solution B divides 2h uniformly to drip
Add, 3h is aged after being added dropwise to complete, then separate solid with solvent, gained solid is automatically cleaning aluminum paste.
Examined through field emission scanning electron microscope and field emission scanning electron microscope energy dispersive spectrometer, find aluminium silver
Starch the fine and close TiO of Surface coating2Film.
Embodiment 3
A kind of automatically cleaning aluminum paste preparation method, is comprised the following steps that:
(1) 1 parts by weight oiliness aluminum paste is mixed with the acetone of 1.5 parts by weight, after certain time by solid mixture with
Solvent separates;
(2) titanate coupling agent isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters are mixed with isopropanol, obtained
The mixed solution A of titanate coupling agent isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters mass fraction 10%;By metatitanic acid
Four butyl esters mix with isopropanol, obtain the mixed solution B of butyl titanate mass fraction 25%;
(3) aluminum paste and the isopropanol of 9 parts by weight crossed acetone treatment, the mixed solution A and 0.1 weight of 1 parts by weight
The water mixing of part is measured, reacts, separates solid mixture after a period of time stand-by under conditions of 60 DEG C;;
(4) solid mixture obtained by step (3) is mixed with the isopropanol of 9 parts by weight and the water of 0.1 parts by weight, uses ammonia
Water adjusts pH to 7, and the mixed solution B of 1 parts by weight is added dropwise under conditions of 60 DEG C, wherein, mixed solution B divides 2h uniformly to drip
Add, 4h is aged after being added dropwise to complete, then separate solid with solvent, gained solid is automatically cleaning aluminum paste.
Examined through field emission scanning electron microscope and field emission scanning electron microscope energy dispersive spectrometer, find aluminium silver
Starch the fine and close TiO of Surface coating2Film.
Embodiment 4
A kind of automatically cleaning aluminum paste preparation method, is comprised the following steps that:
(1) 1 parts by weight oiliness aluminum paste is mixed with the acetone of 3 parts by weight, after certain time by solid mixture with it is molten
Agent separates;
(2) titanate coupling agent Di(dioctylpyrophosphato) ethylene titanate is mixed with isopropanol, obtains titanium
The mixed solution A of acid esters coupling agent Di(dioctylpyrophosphato) ethylene titanate mass fraction 10%;By the fourth of metatitanic acid four
Ester mixes with isopropanol, obtains the mixed solution B of butyl titanate mass fraction 25%;
(3) aluminum paste and the isopropanol of 9 parts by weight crossed acetone treatment, the mixed solution A and 0.1 weight of 1 parts by weight
The water mixing of part is measured, separates solid mixture with solvent after 60 DEG C of reactions;
(4) solid mixture obtained by step (3) is mixed with the isopropanol of 9 parts by weight and the water of 0.1 parts by weight, uses ammonia
Water adjusts pH to 7, and the mixed solution B of 0.5 parts by weight is added dropwise under conditions of 60 DEG C, wherein, mixed solution B divides 2.5h uniform
It is added dropwise, 4h is aged after being added dropwise to complete, then separates solid with solvent, gained solid is automatically cleaning aluminum paste.
Examined through field emission scanning electron microscope and field emission scanning electron microscope energy dispersive spectrometer, find aluminium silver
Starch the fine and close TiO of Surface coating2Film.
Embodiment 5
A kind of automatically cleaning aluminum paste preparation method, is comprised the following steps that:
(1) the commercially available oiliness aluminum paste of 1 parts by weight is mixed with 3 pbw acetones, isolated aluminium silver after certain time
It is stand-by to starch solid;
(2) titanate coupling agent Di(dioctylpyrophosphato) ethylene titanate is mixed with isopropanol, obtains titanium
Acid esters coupling agent Di(dioctylpyrophosphato) ethylene titanate mass fraction is 10% mixed solution A;By metatitanic acid four
Butyl ester mixes with isopropanol, obtains the mixed solution B that butyl titanate mass fraction is 25%;
(3) by the aluminum paste solid obtained by step (1) and the isopropanol of 5 parts by weight, 2 parts by weight mixed solution A and
The water of 0.1 parts by weight is mixed, and is reacted under conditions of 80 DEG C, obtains solid mixture, wherein aluminum paste solid is with mixing
The addition of solution A is to make gained solid mixture and the mass ratio of titanate coupling agent be 1:0.08, will be solid after a period of time
The separation of body mixture is stand-by;
(4) solid mixture obtained by step (3) is mixed with the isopropanol of 5 parts by weight and the water of 0.1 parts by weight, uses ammonia
Water adjusts pH to 8, and mixed solution B is added dropwise under conditions of 80 DEG C, and mixed solution B addition is to make the solid mixture
Mass ratio with butyl titanate is 1:0.5, wherein, mixed solution B divides 1h to be uniformly added dropwise, and 6h is aged after being added dropwise to complete, then
Solid is separated with solvent, gained solid is automatically cleaning aluminum paste.
Examined through field emission scanning electron microscope and field emission scanning electron microscope energy dispersive spectrometer, find aluminium silver
Starch the fine and close TiO of Surface coating2Film.
Embodiment 6
A kind of automatically cleaning aluminum paste preparation method, is comprised the following steps that:
(1) the commercially available oiliness aluminum paste of 1 parts by weight is mixed with 3.5 pbw acetones, isolated aluminium after certain time
Silver paste solid is stand-by;
(2) titanate coupling agent Di(dioctylpyrophosphato) ethylene titanate is mixed with isopropanol, obtains titanium
Acid esters coupling agent Di(dioctylpyrophosphato) ethylene titanate mass fraction is 10% mixed solution A;By metatitanic acid four
Butyl ester mixes with isopropanol, obtains the mixed solution B that butyl titanate mass fraction is 75%;
(3) by the aluminum paste solid and isopropanol of 10 parts by weight obtained by step (1), mixed solution A and 0.1 parts by weight
Water mixed, reacted under conditions of 60 DEG C, obtain solid mixture, wherein aluminum paste solid and mixed solution A adds
Dosage is to make gained solid mixture and the mass ratio of titanate coupling agent be 1:0.2.By solid mixture point after a period of time
From stand-by;
(4) solid mixture obtained by step (3) is mixed with the isopropanol of 10 parts by weight and the water of 0.1 parts by weight, used
Ammoniacal liquor adjusts pH to 7.5, and mixed solution B is added dropwise under conditions of 60 DEG C, and mixed solution B addition is to mix the solid
The mass ratio of compound and butyl titanate is 1:0.25, wherein, mixed solution B divides 1h to be uniformly added dropwise, and 5h is aged after being added dropwise to complete,
Then solid is separated with solvent, gained solid is automatically cleaning aluminum paste.
Examined through field emission scanning electron microscope and field emission scanning electron microscope energy dispersive spectrometer, find aluminium silver
Starch the fine and close TiO of Surface coating2Film.
Claims (7)
1. a kind of automatically cleaning water aluminum-silver slurry, it is characterised in that the water aluminum-silver slurry is aluminum paste Surface coating TiO2Film, lead to
Cross TiO2Automatically cleaning and water solubility are realized in the photocatalysis of film;
Described automatically cleaning water aluminum-silver slurry is made using sol-gal process, specifically includes following steps:
(1) parts by weight of oiliness aluminum paste 1 are mixed with the parts by weight of acetone 1.5~3.5, removes the organic of oiliness aluminum paste surface
Thing, obtain aluminum paste solid;
(2) titanate coupling agent is mixed with organic solvent, obtains mixed solution A, butyl titanate is mixed with organic solvent,
Obtain mixed solution B;
(3) the aluminum paste solid obtained by step (1) and the parts by weight of organic solvent 5~10, mixed solution A, the parts by weight of water 0.1 are entered
Row mixing, isolated solid mixture after 60~80 DEG C of reactions;
(4) solid mixture obtained by step (3) is mixed with the parts by weight of organic solvent 5~10, the parts by weight of water 0.1, adjusts pH to 7
Under the conditions of~8,60~80 DEG C, mixed solution B is added dropwise, ageing, which separates, after reaction produces automatically cleaning water aluminum-silver slurry;
The mass ratio of aluminum paste solid and titanate coupling agent in described step (3) is 1:(0.08-0.2);Described step
Suddenly the mass ratio of the solid mixture in (4) and butyl titanate is 1:(0.25-0.5).
2. a kind of automatically cleaning water aluminum-silver slurry according to claim 1, it is characterised in that step (2), step (3), step
(4) organic solvent described in is ethanol or isopropanol.
A kind of 3. automatically cleaning water aluminum-silver slurry according to claim 1, it is characterised in that the titanate esters described in step (2)
Coupling agent includes chelate solution, the isopropyl three (two of Di(dioctylpyrophosphato) ethylene titanate and triethanolamine
Octyl group pyrophosphoric acid acyloxy) one kind in titanate esters or Di(dioctylpyrophosphato) ethylene titanate.
A kind of 4. automatically cleaning water aluminum-silver slurry according to claim 1, it is characterised in that step (2) described mixed solution A
Mass concentration be 10%;
The mass concentration of the mixed solution B is 25%-75%.
5. a kind of automatically cleaning water aluminum-silver slurry according to claim 1, it is characterised in that be used to adjust pH in step (4)
Conditioning agent be triethylamine or ammoniacal liquor.
A kind of 6. automatically cleaning water aluminum-silver slurry according to claim 1, it is characterised in that mixed solution B in step (4)
Time for adding is 1~5h.
7. a kind of automatically cleaning water aluminum-silver slurry according to claim 1, it is characterised in that digestion time is 3 in step (4)
~6h.
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