CN107325673A - A kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating - Google Patents
A kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating Download PDFInfo
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- CN107325673A CN107325673A CN201710424661.0A CN201710424661A CN107325673A CN 107325673 A CN107325673 A CN 107325673A CN 201710424661 A CN201710424661 A CN 201710424661A CN 107325673 A CN107325673 A CN 107325673A
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- C—CHEMISTRY; METALLURGY
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
- C09D133/16—Homopolymers or copolymers of esters containing halogen atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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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
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3676—Treatment with macro-molecular organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
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- C09D5/1618—Non-macromolecular compounds inorganic
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
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Abstract
The invention discloses a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating, belong to technical field of paint preparation.The present invention first passes through alkali leaching and removes straw lignin, liquid freezes between making fiber through liquid nitrogen frozen, ice crystal phase mutual friction is set to allow fiber tentatively to dissociate by grinding, polyhydroxy fiber powder is obtained with steam blasting again, fiber powder is soaked with dopamine solution, self-polymeric reaction is crosslinked in the presence of dissolved oxygen using dopamine, in fiber powder surface attachment dopamine film, recycle titanium ion in sequestering chelate solution at initial stage of dopamine, through hydrolysis in template surface formation titanium dioxide layer, removing template is calcined again obtains nano titanium oxide, again by after titanium dioxide and natural resin peach gum mixed grinding, it is modified through microorganism, increase the peach gum particle of titanium dioxide ion surface, so as to improve the compatibility between titanium dioxide and coating resin matrix, it is finally reached the purpose for improving coating automatically cleaning effect, have broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating, belong to coating preparation technology neck
Domain.
Background technology
Glass self-cleaning coating is a kind of super-hydrophilic coating for being sprayed on glass surface, coated face and it is dirty between it is rapid
Form one layer of super hydrophilic moisture film, make dirty release-coated face, using nature rainwash, make it is dirty with moisture film gravity work
It is rinsed under, reaches self-cleaning purpose.
It is divided into three classes currently used for the self-cleaning coating of glass surface：One class main component is silicone（Or silicone）Or
The materials of the other oiliness of person is constituted, and is coated in that material surface is glossy, light, but can not be acted on the silicon dioxide molecules of material surface
The firm nano thin-film of generation, and simply filled and led up rough material surface so that material surface smooth even, its advantage
It is to have very strong repulsive interaction to water, has the disadvantage that tack is not good, self-cleaning persistence is short.Two class main components are titanium dioxide
（TiO2）, on glass after plating/painting layer of titanium dioxide film, because titanium dioxide exists（Ultraviolet）Can in the presence of luminous energy
Produce good photocatalysis characteristic and with Superhydrophilic, utilize this super hydrophilic characteristic so that the water droplet of very little is converged to greatly
Water droplet, come off under gravity so that contamination can be readily washed away in spot thereon, have glass
There is characteristic easy to clean, its is cheap, but because nano titanium oxide surface can be high, in non-thermodynamics stable state, easily
The poor compatibility agglomerated between second particle, and nano titanium oxide and coating matrix, causes automatically cleaning effect poor, easy to stick
Ash and absorption oiliness pollutant.Three class main components are inorganic nano silicon materials, are characterized in surface for super-hydrophilic coating and prevent
Dust is good, independent of sunlight irradiation, is worked in the next sample of complete no light conditions, but not rub resistance, short life and not grease proofing.
It would therefore be highly desirable to develop a kind of good tack, self-cleaning persistence length, good automatically cleaning effect, coating rub resistance and use
The glass self-cleaning coating of long lifespan.
The content of the invention
The technical problems to be solved by the invention：For common self-cleaning coating at present using nano titanium oxide to fill out
Material, because nano titanium oxide surface can be high, in non-thermodynamics stable state, easily agglomerates into second particle, and nanometer two
Poor compatibility between titanium oxide and coating matrix, causing the poor defect of automatically cleaning effect, there is provided a kind of nano titanium oxide glass
The preparation method of glass self-cleaning coating.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）Weigh 2~3kg rice straws and crush 20~30min, stalk fragment is obtained, by stalk fragment sodium hydroxide solution
Soak and filtered after 6~8h, isolated filter residue freezes 10~15s of filter residue with liquid nitrogen spraying immediately, and the filter residue after freezing is ground
1~2h, obtains refining stalk wet feed；
（2）Above-mentioned refinement stalk wet feed is subjected to steam blasting, gas explosion material is obtained and dries, obtain polyhydroxy superfine fibre
Powder, then by polyhydroxy superfine fibre powder and mass concentration be that 4g/L dopamine solutions are 1 in mass ratio:After 10 mixing, it is placed on
6~8h of vibration dipping on shaking table, is separated by filtration and obtains impregnating filter residue, as self-control deposition template；
（3）The above-mentioned self-control deposition templates of 2~3g are taken to be scattered in 500~600mL mass fractions in 70% ethanol solution, stirring is mixed
Close, and it is 70% ethanol solution that 10~15mL butyl titanates and 100~150mL mass fractions are added dropwise successively under stirring,
Continue 2~4h of stirring reaction, obtain milky suspension；
（4）Above-mentioned milky suspension is separated by filtration and obtains filter cake, then by filter cake heat preservation sintering, it is cold with stove after terminating
But to room temperature, it is hollow Nano titanium dioxide microballoon sphere to obtain sintered product, then by hollow Nano titanium dioxide microballoon sphere and peach gum
By 10~15min is ground after waiting mass ratio mixing, it is fitted into the mixture after grinding as fermentation substrate in fermentation tank, then to hair
Bacillus subtilis bacteria suspension, sealing and fermenting after being stirred with sterile rod are added in fermentation tank；
（5）After after above-mentioned fermentation ends, tunning is taken out, is separated by filtration and obtains the filter residue that ferments, automatically cleaning filler is as modified,
Count by weight, weigh 15~20 parts of methyl methacrylates and 20~25 parts of hexafluorobutyl acrylates load with agitator
Three-necked flask in, stir to obtain mix monomer, the potassium peroxydisulfate of mix monomer gross mass 0.1~0.3% is added, by flask
Move into 70~80 DEG C of oil bath pans, the polyvinyl alcohol of mix monomer gross mass 3~5% is added dropwise while stirring, be incubated polymerisation 2
~3h, obtains pre-emulsion；
（6）Count by weight, weigh 10~15 parts of above-mentioned modified automatically cleaning fillers, 20~30 parts of deionized waters, 70~80 parts
Above-mentioned pre-emulsion and 2~4 parts of Lauryl Alcohol esters are poured into colloid mill successively, after 3~5h of grinding, and discharge tinning, produces nanometer two
Titania glass self-cleaning coating.
Step（1）Described in stalk fragment and sodium hydroxide solution mass ratio be 1:5, the concentration of sodium hydroxide solution
For 1mol/L.
Described refinement stalk wet feed steam blasting operating process is：Stalk wet feed will be refined and load steam blasting device
In gas explosion tank, and be passed through into gas explosion tank and be preheated to 200~220 DEG C of water vapour, until in gas explosion tank pressure reach 2.3~
After 2.5MPa, 1~2min of pressurize, gas explosion tank outlet valve is opened, the material moment in gas explosion tank is ejected, obtains gas explosion thing
Material.
Described heat preservation sintering temperature is 600~700 DEG C, and the heat preservation sintering time is 1~2h.
Step（4）Described in bacillus subtilis bacteria suspension concentration be 105cfu/mL, bacillus subtilis bacteria suspension
Addition be fermentation substrate quality 10%, fermentation time be 7~10 days.
The present invention is compared with other method, and advantageous effects are：
（1）The present invention soaks the lignin removed in stalk by alkali first, interfibrous liquid is frozen through liquid nitrogen frozen, freezes
Process liquids volume become big, strutting fiber makes it into swelling state, then phase mutual friction is allowed fiber by grinding
Preliminary dissociation, then polyhydroxy fiber powder is obtained with steam blasting, fiber powder then is soaked with dopamine solution, is existed using dopamine
Self-polymeric reaction is crosslinked in the presence of oxygen in water, the compound poly-dopamine film of strength attachment is formed on fiber powder surface
Layer, recycles titanium ion in sequestering chelate solution at initial stage of dopamine film layer, through hydrolysis in template surface formation dioxy
Change titanium layer, titanium dioxide uniform ion is distributed in template surface, it is to avoid the generation of agglomeration；
（2）Last calcining of the invention goes removing template to obtain nano titanium oxide, then titanium dioxide and natural resin peach gum are mixed
After grinding, it is modified through microorganism, increases the peach gum particle of titanium dioxide ion surface, using between natural resin and coating resin
Excellent compatibility improves the purpose of the compatibility between titanium dioxide and coating resin matrix to reach, is finally reached raising coating certainly
The purpose of cleaning effect, has broad application prospects.
Embodiment
2~3kg rice straws are weighed first, are put into 20~30min of crushing in airslide disintegrating mill, are obtained stalk fragment, will
Stalk fragment and concentration are that 1mol/L sodium hydroxide solutions are 1 in mass ratio:Filtered after 5 mixing, 6~8h of immersion, it is isolated
Filter residue, freezes 10~15s of filter residue with liquid nitrogen spraying immediately, and the filter residue after freezing is moved into mortar, grinds 1~2h, is refined
Stalk wet feed；Refinement stalk wet feed is fitted into the gas explosion tank of steam blasting device, and be passed through into gas explosion tank be preheated to 200~
220 DEG C of water vapour, until pressure is reached after 2.3~2.5MPa, 1~2min of pressurize in gas explosion tank, opens gas explosion tank outlet valve,
The material moment in gas explosion tank is set to be injected into reception kettle；Take out material in reception kettle and be transferred to baking oven, at 105~110 DEG C
1~2h is dried, polyhydroxy superfine fibre powder is obtained, then by polyhydroxy superfine fibre powder and mass concentration is 4g/L dopamine solutions
It is 1 in mass ratio:After 10 mixing, 6~8h of vibration dipping on shaking table is placed on, is separated by filtration and obtains impregnating filter residue, as make by oneself
Deposit template；Then 2~3g self-control deposition templates are taken to be scattered in equipped with the burning that 500~600mL mass fractions are 70% ethanol solution
In cup, beaker is placed on magnetic stirrer, is stirred with 300~400r/min rotating speeds, to beaker under stirring
In 10~15mL butyl titanates and 100~150mL mass fractions are added dropwise successively is 70% ethanol solution, reduction speed of agitator is extremely
100~150r/min, continues 2~4h of stirring reaction, obtains milky suspension；Milky suspension is separated by filtration again and obtained
Filter cake, then filter cake is put into tube type resistance furnace, 1~2h of heat preservation sintering at 600~700 DEG C, after terminating, it will be produced in stove
Thing cools to room temperature with the furnace, takes out and can obtain hollow Nano titanium dioxide microballoon sphere；By hollow Nano titanium dioxide microballoon sphere and peach
Glue is put into 10~15min of grinding in ball grinder, the mixture after grinding is loaded as fermentation substrate by waiting after mass ratio mixing
In fermentation tank, then it is 10 to add the concentration of fermentation substrate quality 10% into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions,
Sealing and fermenting 7~10 days after being stirred with sterile rod；After after fermentation ends, tunning is taken out, is separated by filtration and is fermented
Filter residue, is as modified automatically cleaning filler, counts by weight, weigh 15~20 parts of methyl methacrylates and 20~25 parts of propylene
Sour hexafluoro butyl ester is fitted into the three-necked flask with agitator, and stir to obtain mix monomer, adds mix monomer gross mass
0.1~0.3% potassium peroxydisulfate, flask is moved into 70~80 DEG C of oil bath pans, and mix monomer gross mass 3~5% is added dropwise while stirring
Polyvinyl alcohol, be incubated 2~3h of polymerisation, obtain pre-emulsion；Finally count by weight, weigh 10~15 parts of modifications from clear
Clean filler, 20~30 parts of deionized waters, 70~80 parts of pre-emulsions and 2~4 parts of Lauryl Alcohol esters are poured into colloid mill successively, grinding
After 3~5h, discharge tinning, produces nanometer titanium dioxide titanium glass self-cleaning coating.
Example 1
2kg rice straws are weighed first, is put into airslide disintegrating mill and crushes 20min, stalk fragment is obtained, by stalk fragment and dense
Degree is that 1mol/L sodium hydroxide solutions are 1 in mass ratio:Filtered after 5 mixing, immersion 6h, isolated filter residue uses liquid nitrogen immediately
Spray refrigeration filter residue 10s, mortar is moved into by the filter residue after freezing, grinds 1h, obtains refining stalk wet feed；Stalk wet feed will be refined
It is fitted into the gas explosion tank of steam blasting device, and is passed through into gas explosion tank and is preheated to 200 DEG C of water vapour, until is pressed in gas explosion tank
Power is reached after 2.3MPa, pressurize 1min, is opened gas explosion tank outlet valve, the material moment in gas explosion tank is injected into reception kettle
In；Take out material in reception kettle and be transferred to baking oven, 1h is dried at 105 DEG C, polyhydroxy superfine fibre powder is obtained, then polyhydroxy is surpassed
Fine fibre powder and mass concentration are that 4g/L dopamine solutions are 1 in mass ratio:After 10 mixing, it is placed on shaking table and vibrates dipping
6h, is separated by filtration and obtains impregnating filter residue, as self-control deposition template；Then 2g self-control deposition templates are taken to be scattered in equipped with 500mL
Mass fraction for 70% ethanol solution beaker in, beaker is placed on magnetic stirrer, stirred with 300r/min rotating speeds
Mix, it is 70% ethanol solution, drop that 10mL butyl titanates and 100mL mass fractions are added dropwise successively into beaker under stirring
Low speed of agitator continues stirring reaction 2h, obtains milky suspension to 100r/min；Milky suspension is separated by filtration again
Obtain filter cake, then filter cake be put into tube type resistance furnace, the heat preservation sintering 1h at 600 DEG C, after terminating, by product in stove with
Stove is cooled to room temperature, takes out and can obtain hollow Nano titanium dioxide microballoon sphere；Hollow Nano titanium dioxide microballoon sphere and peach gum are pressed
After mass ratio mixing, it is put into ball grinder and grinds 10min, loads fermentation tank using the mixture after grinding as fermentation substrate
In, then it is 10 to add the concentration of fermentation substrate quality 10% into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions, with sterile
Sealing and fermenting 7 days after rod stirs；After after fermentation ends, tunning is taken out, is separated by filtration and obtains the filter residue that ferments, as change
Property automatically cleaning filler, count by weight, weigh 15 parts of methyl methacrylates and 20 parts of hexafluorobutyl acrylates load and carried
In the three-necked flask of agitator, stir to obtain mix monomer, the potassium peroxydisulfate of mix monomer gross mass 0.1% is added, by flask
Move into 70 DEG C of oil bath pans, the polyvinyl alcohol of mix monomer gross mass 3% is added dropwise while stirring, be incubated polymerisation 2h, obtain pre-
Emulsion；Finally count by weight, weigh 10 parts of modified automatically cleaning fillers, 20 parts of deionized waters, 70 parts of pre-emulsions and 2 part 12
Carbon alcohol ester is poured into colloid mill successively, after grinding 3h, and discharge tinning, produces nanometer titanium dioxide titanium glass self-cleaning coating.
It is first that glass surface dust, cleaning oil pollution is clean, then rinsed 2 times with clear water, and wiped 2 times with rag, wipe
Into, nanometer titanium dioxide titanium glass self-cleaning coating produced by the present invention is fitted into spray gun, uniformly sprayed in glass surface, control
Thickness is sprayed for 15 μm, after the completion of spraying, solidification 28h is stood.Self-cleaning coating of the present invention is strong with glass surface adhesive force,
The spot on glass can be effectively decomposed by the photocatalysis of nano titanium oxide, self-cleaning effect is played, at the same have compared with
Good dirt-resistant ability, using rear glass surface light transmittance up to 89.8%, rear glass surface is used than Conventional nano self-cleaning coating
Light transmittance（85.7%）Rise 4.1%.
Example 2
3kg rice straws are weighed first, is put into airslide disintegrating mill and crushes 25min, stalk fragment is obtained, by stalk fragment and dense
Degree is that 1mol/L sodium hydroxide solutions are 1 in mass ratio:Filtered after 5 mixing, immersion 7h, isolated filter residue uses liquid nitrogen immediately
Spray refrigeration filter residue 13s, mortar is moved into by the filter residue after freezing, grinds 2h, obtains refining stalk wet feed；Stalk wet feed will be refined
It is fitted into the gas explosion tank of steam blasting device, and is passed through into gas explosion tank and is preheated to 210 DEG C of water vapour, until is pressed in gas explosion tank
Power is reached after 2.4MPa, pressurize 2min, is opened gas explosion tank outlet valve, the material moment in gas explosion tank is injected into reception kettle
In；Take out material in reception kettle and be transferred to baking oven, 2h is dried at 108 DEG C, polyhydroxy superfine fibre powder is obtained, then polyhydroxy is surpassed
Fine fibre powder and mass concentration are that 4g/L dopamine solutions are 1 in mass ratio:After 10 mixing, it is placed on shaking table and vibrates dipping
7h, is separated by filtration and obtains impregnating filter residue, as self-control deposition template；Then 3g self-control deposition templates are taken to be scattered in equipped with 550mL
Mass fraction for 70% ethanol solution beaker in, beaker is placed on magnetic stirrer, stirred with 350r/min rotating speeds
Mix, it is 70% ethanol solution, drop that 13mL butyl titanates and 130mL mass fractions are added dropwise successively into beaker under stirring
Low speed of agitator continues stirring reaction 3h, obtains milky suspension to 130r/min；Milky suspension is separated by filtration again
Obtain filter cake, then filter cake be put into tube type resistance furnace, the heat preservation sintering 2h at 650 DEG C, after terminating, by product in stove with
Stove is cooled to room temperature, takes out and can obtain hollow Nano titanium dioxide microballoon sphere；Hollow Nano titanium dioxide microballoon sphere and peach gum are pressed
After mass ratio mixing, it is put into ball grinder and grinds 13min, loads fermentation tank using the mixture after grinding as fermentation substrate
In, then it is 10 to add the concentration of fermentation substrate quality 10% into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions, with sterile
Sealing and fermenting 8 days after rod stirs；After after fermentation ends, tunning is taken out, is separated by filtration and obtains the filter residue that ferments, as change
Property automatically cleaning filler, count by weight, weigh 18 parts of methyl methacrylates and 23 parts of hexafluorobutyl acrylates load and carried
In the three-necked flask of agitator, stir to obtain mix monomer, the potassium peroxydisulfate of mix monomer gross mass 0.2% is added, by flask
Move into 75 DEG C of oil bath pans, the polyvinyl alcohol of mix monomer gross mass 4% is added dropwise while stirring, be incubated polymerisation 3h, obtain pre-
Emulsion；Finally count by weight, weigh 13 parts of modified automatically cleaning fillers, 25 parts of deionized waters, 75 parts of pre-emulsions and 3 part 12
Carbon alcohol ester is poured into colloid mill successively, after grinding 4h, and discharge tinning, produces nanometer titanium dioxide titanium glass self-cleaning coating.
It is first that glass surface dust, cleaning oil pollution is clean, then rinsed 3 times with clear water, and wiped 2 times with rag, wipe
Into, nanometer titanium dioxide titanium glass self-cleaning coating produced by the present invention is fitted into spray gun, uniformly sprayed in glass surface, control
Thickness is sprayed for 18 μm, after the completion of spraying, solidification 38h is stood.Self-cleaning coating of the present invention is strong with glass surface adhesive force,
The spot on glass can be effectively decomposed by the photocatalysis of nano titanium oxide, self-cleaning effect is played, at the same have compared with
Good dirt-resistant ability, using rear glass surface light transmittance up to 91.9%, rear glass surface is used than Conventional nano self-cleaning coating
Light transmittance（83.6%）Rise 8.3%.
Example 3
3kg rice straws are weighed first, is put into airslide disintegrating mill and crushes 30min, stalk fragment is obtained, by stalk fragment and dense
Degree is that 1mol/L sodium hydroxide solutions are 1 in mass ratio:Filtered after 5 mixing, immersion 8h, isolated filter residue uses liquid nitrogen immediately
Spray refrigeration filter residue 15s, mortar is moved into by the filter residue after freezing, grinds 2h, obtains refining stalk wet feed；Stalk wet feed will be refined
It is fitted into the gas explosion tank of steam blasting device, and is passed through into gas explosion tank and is preheated to 220 DEG C of water vapour, until is pressed in gas explosion tank
Power is reached after 2.5MPa, pressurize 2min, is opened gas explosion tank outlet valve, the material moment in gas explosion tank is injected into reception kettle
In；Take out material in reception kettle and be transferred to baking oven, 2h is dried at 110 DEG C, polyhydroxy superfine fibre powder is obtained, then polyhydroxy is surpassed
Fine fibre powder and mass concentration are that 4g/L dopamine solutions are 1 in mass ratio:After 10 mixing, it is placed on shaking table and vibrates dipping
8h, is separated by filtration and obtains impregnating filter residue, as self-control deposition template；Then 3g self-control deposition templates are taken to be scattered in equipped with 600mL
Mass fraction for 70% ethanol solution beaker in, beaker is placed on magnetic stirrer, stirred with 400r/min rotating speeds
Mix, it is 70% ethanol solution, drop that 15mL butyl titanates and 150mL mass fractions are added dropwise successively into beaker under stirring
Low speed of agitator continues stirring reaction 4h, obtains milky suspension to 150r/min；Milky suspension is separated by filtration again
Obtain filter cake, then filter cake be put into tube type resistance furnace, the heat preservation sintering 2h at 700 DEG C, after terminating, by product in stove with
Stove is cooled to room temperature, takes out and can obtain hollow Nano titanium dioxide microballoon sphere；Hollow Nano titanium dioxide microballoon sphere and peach gum are pressed
After mass ratio mixing, it is put into ball grinder and grinds 15min, loads fermentation tank using the mixture after grinding as fermentation substrate
In, then it is 10 to add the concentration of fermentation substrate quality 10% into fermentation tank5Cfu/mL bacillus subtilis bacteria suspensions, with sterile
Sealing and fermenting 10 days after rod stirs；After after fermentation ends, tunning is taken out, is separated by filtration and obtains the filter residue that ferments, is
Modified automatically cleaning filler, is counted by weight, weighs 20 parts of methyl methacrylates and 25 parts of hexafluorobutyl acrylates load band
Have in the three-necked flask of agitator, stir to obtain mix monomer, add the potassium peroxydisulfate of mix monomer gross mass 0.3%, will burn
Bottle is moved into 80 DEG C of oil bath pans, and the polyvinyl alcohol of mix monomer gross mass 5% is added dropwise while stirring, is incubated polymerisation 3h, is obtained
Pre-emulsion；Finally count by weight, weigh 15 parts of modified automatically cleaning fillers, 30 parts of deionized waters, 80 parts of pre-emulsions and 4 part ten
Two carbon alcohol esters are poured into colloid mill successively, after grinding 5h, and discharge tinning, produces nanometer titanium dioxide titanium glass self-cleaning coating.
It is first that glass surface dust, cleaning oil pollution is clean, then rinsed 3 times with clear water, and wiped 3 times with rag, wipe
Into, nanometer titanium dioxide titanium glass self-cleaning coating produced by the present invention is fitted into spray gun, uniformly sprayed in glass surface, control
Thickness is sprayed for 20 μm, after the completion of spraying, solidification 48h is stood.Self-cleaning coating of the present invention is strong with glass surface adhesive force,
The spot on glass can be effectively decomposed by the photocatalysis of nano titanium oxide, self-cleaning effect is played, at the same have compared with
Good dirt-resistant ability, using rear glass surface light transmittance up to 93.6%, rear glass surface is used than Conventional nano self-cleaning coating
Light transmittance（81.5%）Rise 12.1%.
Claims (5)
1. a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating, it is characterised in that specifically preparation process is：
（1）Weigh 2~3kg rice straws and crush 20~30min, stalk fragment is obtained, by stalk fragment sodium hydroxide solution
Soak and filtered after 6~8h, isolated filter residue freezes 10~15s of filter residue with liquid nitrogen spraying immediately, and the filter residue after freezing is ground
1~2h, obtains refining stalk wet feed；
（2）Above-mentioned refinement stalk wet feed is subjected to steam blasting, gas explosion material is obtained and dries, obtain polyhydroxy superfine fibre
Powder, then by polyhydroxy superfine fibre powder and mass concentration be that 4g/L dopamine solutions are 1 in mass ratio:After 10 mixing, it is placed on
6~8h of vibration dipping on shaking table, is separated by filtration and obtains impregnating filter residue, as self-control deposition template；
（3）The above-mentioned self-control deposition templates of 2~3g are taken to be scattered in 500~600mL mass fractions in 70% ethanol solution, stirring is mixed
Close, and it is 70% ethanol solution that 10~15mL butyl titanates and 100~150mL mass fractions are added dropwise successively under stirring,
Continue 2~4h of stirring reaction, obtain milky suspension；
（4）Above-mentioned milky suspension is separated by filtration and obtains filter cake, then by filter cake heat preservation sintering, it is cold with stove after terminating
But to room temperature, it is hollow Nano titanium dioxide microballoon sphere to obtain sintered product, then by hollow Nano titanium dioxide microballoon sphere and peach gum
By 10~15min is ground after waiting mass ratio mixing, it is fitted into the mixture after grinding as fermentation substrate in fermentation tank, then to hair
Bacillus subtilis bacteria suspension, sealing and fermenting after being stirred with sterile rod are added in fermentation tank；
（5）After after above-mentioned fermentation ends, tunning is taken out, is separated by filtration and obtains the filter residue that ferments, automatically cleaning filler is as modified,
Count by weight, weigh 15~20 parts of methyl methacrylates and 20~25 parts of hexafluorobutyl acrylates load with agitator
Three-necked flask in, stir to obtain mix monomer, the potassium peroxydisulfate of mix monomer gross mass 0.1~0.3% is added, by flask
Move into 70~80 DEG C of oil bath pans, the polyvinyl alcohol of mix monomer gross mass 3~5% is added dropwise while stirring, be incubated polymerisation 2
~3h, obtains pre-emulsion；
（6）Count by weight, weigh 10~15 parts of above-mentioned modified automatically cleaning fillers, 20~30 parts of deionized waters, 70~80 parts
Above-mentioned pre-emulsion and 2~4 parts of Lauryl Alcohol esters are poured into colloid mill successively, after 3~5h of grinding, and discharge tinning, produces nanometer two
Titania glass self-cleaning coating.
2. a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating according to claim 1, it is characterised in that：
Step（1）Described in stalk fragment and sodium hydroxide solution mass ratio be 1:5, the concentration of sodium hydroxide solution is 1mol/
L。
3. a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating according to claim 1, it is characterised in that：
Described refinement stalk wet feed steam blasting operating process is：The gas explosion tank of stalk wet feed loading steam blasting device will be refined
In, and be passed through into gas explosion tank and be preheated to 200~220 DEG C of water vapour, until pressure reaches 2.3~2.5MPa in gas explosion tank,
After 1~2min of pressurize, gas explosion tank outlet valve is opened, the material moment in gas explosion tank is ejected, obtains gas explosion material.
4. a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating according to claim 1, it is characterised in that：
Described heat preservation sintering temperature is 600~700 DEG C, and the heat preservation sintering time is 1~2h.
5. a kind of preparation method of nanometer titanium dioxide titanium glass self-cleaning coating according to claim 1, it is characterised in that：
Step（4）Described in bacillus subtilis bacteria suspension concentration be 105Cfu/mL, the addition of bacillus subtilis bacteria suspension
For the 10% of fermentation substrate quality, fermentation time is 7~10 days.
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| CN108822342A (en) * | 2018-06-12 | 2018-11-16 | 阜南县胜天新能源开发有限公司 | A kind of preparation method of straw charcoal plastic filler |
| CN109177563A (en) * | 2018-08-17 | 2019-01-11 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of blotting material |
| CN109439087A (en) * | 2018-10-10 | 2019-03-08 | 宁波革创新材料科技有限公司 | The preparation method of high rigidity powdery paints with antibiotic property |
| CN112552045A (en) * | 2020-12-28 | 2021-03-26 | 海宁拓材科技股份有限公司 | Low-valence zirconia optical coating material and preparation method thereof |
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| CN106185952A (en) * | 2016-06-30 | 2016-12-07 | 宁波江东索雷斯电子科技有限公司 | A kind of method utilizing rice husk to prepare high dispersancy nano white carbon |
| CN106366826A (en) * | 2016-08-31 | 2017-02-01 | 浙江润阳新材料科技股份有限公司 | Nano-TiO2 self-cleaning coating and preparation method thereof |
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| CN108822342A (en) * | 2018-06-12 | 2018-11-16 | 阜南县胜天新能源开发有限公司 | A kind of preparation method of straw charcoal plastic filler |
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| CN113652071A (en) * | 2021-09-23 | 2021-11-16 | 深圳市金诚载带有限公司 | Moisture-proof and anti-aging PC carrier tape material and preparation method thereof |
| CN113652071B (en) * | 2021-09-23 | 2023-03-07 | 深圳市金诚载带有限公司 | Moisture-proof and anti-aging PC carrier tape material and preparation method thereof |
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