CN108441091A - A kind of photocatalyst urges the preparation method of dry Polyester Paint - Google Patents
A kind of photocatalyst urges the preparation method of dry Polyester Paint Download PDFInfo
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- CN108441091A CN108441091A CN201810371615.3A CN201810371615A CN108441091A CN 108441091 A CN108441091 A CN 108441091A CN 201810371615 A CN201810371615 A CN 201810371615A CN 108441091 A CN108441091 A CN 108441091A
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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
- 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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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
- 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
- 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
- C09D5/1687—Use of special additives
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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
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; DRIERS (SICCATIVES); TURPENTINE
- C09F9/00—Compounds to be used as driers (siccatives)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/04—Polymer mixtures characterised by other features containing interpenetrating networks
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses the preparation methods that a kind of photocatalyst urges dry Polyester Paint, belong to technical field of paint preparation.Epoxidized soybean oil has stronger antioxygenic property in acrylic acid ester emulsion of the present invention,And the solidification of Polyester Paint can be crosslinked and play facilitation,With acrylate hydroxyl condensation dehydration occurs for epoxidized soybean oil to form network interpenetrating cross-linked structure in the present invention,Contain epoxy group in epoxidized soybean oil,Ehter bond,Hydroxyl isopolarity group and activity group,It and titanium dioxide are combined and is prepared into photocatalyst and urges dry powder,Synergistic effect and photosensitization occur between carbon nanotube and titania molecule,The photocatalytic activity of nano-titanium dioxide can be improved,Improve photocatalysis efficiency,Enhance degradation and volatilization of the titanium dioxide to the solvent of pollution,Play the role of urging dry,And the toxic and harmful gas such as formaldehyde in air of effectively degrading,Various bacteria can effectively be killed,Polyester paint film is also set to have deodorization,Antifouling property,It has a extensive future.
Description
Technical field
The invention discloses the preparation methods that a kind of photocatalyst urges dry Polyester Paint, belong to technical field of paint preparation.
Background technology
Polyester Paint is also unsaturated polyester varnish, it is a kind of multicomponent paint, is made of main film forming matter with polyester resin
A kind of thick matter paint.The paint film of polyester paint is plentiful, and thickness face is hard.Polyester paint equally possesses varnish kind, is polyester varnish.Polyester
Cured in paint work progress, the deal of these curing agent accounts for painting total deal one third.The paint film of Polyester Paint
Excellent combination property makes the hardness higher of paint film because there is the use of curing agent, and hard wear resistant, richness is high, and wet-heat resisting is done
Heat, soda acid oil, solvent and a variety of chemicals, insulating properties are very high.
Into 20th century, the theoretical foundation of polymer science and succeeding in developing for various high-molecular compounds are developed for paint
The new era is started.People have deepened understanding according to macromolecule theory to paint, and paint is not only the mankind and applies earliest one kind
High molecular material, and be the characteristic high molecular material of tool.The exploitation new results of high-molecular compound are utilized in paint extensively,
Using the converted products of various natural high polymers and artificial synthesized synthetic resin as film forming matter, it is excellent to develop multiple performance
Kind expands important function of the paint in human social development.After the incoming China of Polyester Paint, quickly just instead of varnish,
As the main paint of furniture.There are many advantages of Polyester Paint, not only color very abundant, but also film thickness is big, spraying two
Three times, and can completely the material of base cover, so do furniture can in density board direct brush Polyester Paint
, the requirement to base material is high.The flexibility of saturated polyester paint is poor, and embrittlement is easy when stress, once paint film is impaired not
Protection furniture is should be noted that when easily repairing, therefore moving.
It is film forming matter that Polyester Paint, which is with polyester resin, manufactured varnish and enamel paint.In the 1990s, Polyester Paint is passed to me
State becomes the main paint of Furniture manufacturing quickly instead of the varnish of other kinds.Mainly have on Coating Market at present aqueous
Paint and Polyester Paint (oil paint) two types.Water paint adopts water as solvent, and Polyester Paint is using toluene, dimethylbenzene, vinegar class, ketone
Class etc. is solvent.Although the performance of Polyester Paint is higher than water paint, because curing agent used by current Polyester Paint includes
There are the noxious materials such as aromatic isocyanate, such as TDI, uses toluene, dimethylbenzene, vinegar class, ketone etc. for solvent, be easy to make
Pollution at environment and the murder by poisoning for human body.And by ultraviolet illumination Yellowing is easily occurred for paint film for a long time.Therefore, it invents
A kind of photocatalyst urges dry Polyester Paint to have positive effect to technical field of paint preparation.
Invention content
Present invention mainly solves the technical issues of, it is poor for the flexibility of current saturated polyester paint, embrittlement is easy when stress,
It is not easily repaired once paint film is impaired, the Toxics such as aromatic isocyanate, such as TDI is contained in curing agent used by Polyester Paint
Matter, solvent for use are the substances such as toluene, dimethylbenzene, aldoketones, be easy to cause environmental pollution and generate murder by poisoning to human body, and paint
The defect of Yellowing is easily occurred by ultraviolet illumination for a long time for film, provides the preparation method that a kind of photocatalyst urges dry Polyester Paint.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of photocatalyst urges the preparation method of dry Polyester Paint, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, to blender, reflux condensing tube, thermometer, dropping funel four-hole boiling flask in be added 50
~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates start blender with 200~220r/min
Rotating speed stirring, warming-in-water after three-necked flasks are added in 40~45 parts of acrylic acid, 20~30 parts of methacrylic acids, continues anti-
It should obtain seed emulsion；
（2）It counts in parts by weight, 20~30 parts of epoxidized soybean oils is added into above-mentioned three-necked flask, then with dropping funel to four mouthfuls
1~3 part of potassium peroxydisulfate is added dropwise in drop rate in flask, and after being added dropwise, insulation reaction continues heat temperature raising, after insulation reaction
Cooling adjusts pH with ammonium hydroxide, and discharging obtains acrylic acid ester emulsion；
（3）40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and 2~3g carbon nanotubes, ultrasonic disperse obtain carbon nanotube
Carbon nano tube suspension is placed in the three-necked flask with blender and dropping funel by suspension, and speed is added dropwise with dropping funel
18~20mL butyl titanates are added into three-necked flask for rate, while starting blender, are started with the rotating speed of 200~300r/min
10~15min of stirring obtains mixed liquor；
（4）4~5mL acetic acid solutions are added into above-mentioned mixed liquor, 20~30mL silicon dioxide gels stir 1~2h, obtain carbon
Nanotube/TiO 2 sol, it is still aging to obtain dry colloidal sol, dry colloidal sol is placed in baking oven, it is dry, gel piece is obtained, it will
Gel piece is put into mortar and grinds, and sieving obtains photocatalyst and urges dry powder；
（5）It counts in parts by weight, 40~50 parts of asphalt, 10~15 parts of atoleines is placed in stirred tank, heating rises
Temperature, insulated and stirred, then 10~15 parts of nitrile rubber powders are added into stirred tank, continue to stir, obtain modified pitch, gained is modified
Pitch is put into oil bath pan, heat temperature raising, heat preservation, and 10~12 parts of dihydromethyl propionic acids, 8~10 parts of second two are added to oil bath pan
Alcohol, 15~20 parts of toluene, insulation reaction obtain carboxylated pitch；
（6）It counts in parts by weight, by 30~40 parts of M-phthalic acids, 20~25 parts of neopentyl glycols, 5~10 parts of trihydroxy methyls third
Alkane, the mixing of 1~3 part of Mono-n-butyltin, are put into the four-hole boiling flask equipped with condensing unit, start blender, with 400~
The rotating speed of 450r/min stirs, heat temperature raising, under nitrogen protection, 10~15 parts of Isosorbide-5-Nitraes-hexamethylene diformazan is added after insulation reaction
Acid, 4~5 parts of carboxylated pitches, acidolysis reaction are cooled to room temperature, mix 20~30 parts of benzoyl peroxide methyl ethyl ketone, 10~12 parts of light
Catalyst urges dry powder, and the reaction was continued, obtains photocatalyst and urges dry Polyester Paint.
Step（1）Temperature is 70~80 DEG C after the warming-in-water, reacts 10~15min.
Step（2）The dropping funel drop rate is 3~5mL/min, and the insulation reaction time is 30~40min, after
Temperature is 90~100 DEG C after continuous heat temperature raising, and the insulation reaction time is 45~55min, and temperature is 55~60 DEG C after cooling, ammonium hydroxide
Mass fraction 20%, ammonium hydroxide adjust pH be 6.0~7.0.
Step（3）The control supersonic frequency is 30~35kHz, and the ultrasonic disperse time is 4~6min, dropping funel drop
2~3mL/min of rate of acceleration.
Step（4）The mass fraction of the acetic acid solution is 20%, and the still aging time is 2~3 days, baking oven setting temperature
Degree is 60~70 DEG C, and drying time is 10~12h, and milling time is 30~35min, and be sieved specification is 200 mesh.
Step（5）Temperature is 90~100 DEG C after the heat temperature raising, and temperature is 200~220 after oil bath pan heat temperature raising
DEG C, soaking time is 10~15min.
Step（6）Temperature is 230~250 DEG C after the four-hole boiling flask heat temperature raising, under nitrogen protection insulation reaction
Time is 2~3h, and the acidolysis reaction time is 2~3h, continues the reaction time after being cooled to room temperature as 20~30min.
The beneficial effects of the invention are as follows：
（1）The objects such as distilled water, dodecyl sodium sulfate, sodium bicarbonate are added using acrylic acid, methacrylic acid as monomer in the present invention
Seed emulsion is obtained by the reaction by heating stirring in matter, and epoxidized soybean oil is added into seed emulsion, and initiator is anti-by being crosslinked
Ying Houzai adjusts pH with ammonium hydroxide, obtains acrylic acid ester emulsion, is added after carbon nano tube suspension and tetraethyl titanate are mixed a small amount of
Acetic acid and silicon dioxide gel, obtain carbon nano-tube/titanic oxide colloidal sol, be ground up, sieved to obtain after dry photocatalyst urge it is dry
M-phthalic acid, neopentyl glycol, trimethylolpropane are finally mixed, are catalyzed and are caused with Mono-n-butyltin, by poly- by powder
It closes, be added cyclohexane cyclohexanedimethanodibasic after acidolysis, carboxylated pitch, benzoyl peroxide methyl ethyl ketone, photocatalyst urges dry powder to obtain photocatalyst and urge
Dry Polyester Paint, epoxidized soybean oil has stronger antioxygenic property in acrylic acid ester emulsion of the present invention, and can be to Polyester Paint
Facilitation is played in solidification crosslinking, and the increase of the degree of cross linking makes Polyester Paint degradation capability in extraneous aging decline, and photocatalyst is urged dry
Powder utilizes ultraviolet radiation absorption, plays the role of urging dry Polyester Paint and degradating pollution solvent, while can reduce the xanthochromia of paint film
Phenomenon, and decarboxylation occurs with Polyester Paint using carboxylated pitch and polymerize, it improves Polyester Paint and cures rear surface toughness, make Polyester Paint
Film is not easy embrittlement；
（2）With acrylate hydroxyl condensation dehydration occurs for epoxidized soybean oil to form network interpenetrating crosslinking knot in the present invention
Structure contains epoxy group, ehter bond, hydroxyl isopolarity group and activity group in epoxidized soybean oil, makes acrylate glue table
Reveal excellent adhesive strength, improves the adhesive force of Polyester Paint, phenyl ring, which assigns glue heat resistance and rigidity, epoxy group and hydroxyl, to be made
There is material reactivity adhesion strength, the dehydrating condensation of multiple hydroxyls crosslink density to be made to increase, its film-forming efficiency is made to accelerate,
The use of aromatic isocyanate curing agent is reduced, in addition, sorbing material of the carbon nanotube as volatile organic contaminant, by
There is special pipeline configuration in carbon nanotube, lead electronic capability and high-specific surface area, therefore carbon nanotube is to volatile gas
The organic matter of form has very strong adsorption capacity, it and titanium dioxide are combined and is prepared into photocatalyst and urges dry powder, carbon nanotube
Synergistic effect and photosensitization occur between titania molecule, the photocatalytic activity of nano-titanium dioxide can be improved, carbon is received
Receptor of the mitron as electronics is easy to receive the light induced electron that titanium dioxide generates, to effectively inhibit light induced electron and sky
Cave it is compound, improve photocatalysis efficiency, degradation and volatilization of the enhancing titanium dioxide to the solvent of pollution, play the role of urging it is dry,
And effectively degradation toxic and harmful gas such as formaldehyde in air, can effectively kill various bacteria, also make polyester paint film have deodorization,
Antifouling property has a extensive future.
Specific implementation mode
Count in parts by weight, to blender, reflux condensing tube, thermometer, dropping funel four-hole boiling flask in be added
50~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates start blender with 200~220r/
The rotating speed of min stirs, and warming-in-water is added three mouthfuls to 70~80 DEG C, by 40~45 parts of acrylic acid, 20~30 parts of methacrylic acids
After flask, the reaction was continued 10~15min obtains seed emulsion；It counts in parts by weight, 20~30 is added into above-mentioned three-necked flask
Part epoxidized soybean oil, then 1~3 part of potassium peroxydisulfate is added dropwise with 3~5mL/min drop rates into four-hole boiling flask with dropping funel,
After being added dropwise, 30~40min of insulation reaction continues to be heated to 90~100 DEG C, and 45~55min of insulation reaction is cooled to
55~60 DEG C, it is 6.0~7.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylic acid ester emulsion；To ultrasonic disperse
It is added 40~50mL absolute ethyl alcohols and 2~3g carbon nanotubes in instrument, control supersonic frequency is 30~35kHz, ultrasonic disperse 4~
6min obtains carbon nano tube suspension, and carbon nano tube suspension is placed in the three-necked flask with blender and dropping funel,
18~20mL butyl titanates are added into three-necked flask with the drop rate of 2~3mL/min with dropping funel, while starting and stirring
Device is mixed, starting 10~15min of stirring with the rotating speed of 200~300r/min obtains mixed liquor；Into above-mentioned mixed liquor be added 4~
The acetic acid solution that 5mL mass fractions are 20%, 20~30mL silicon dioxide gels stir 1~2h, obtain carbon nanotube/titanium dioxide
Titanium colloidal sol still aging 2~3 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 60~70 DEG C, dry
10~12h obtains gel piece, and gel piece is put into mortar 30~35min of grinding, crosses 200 mesh and sieves to obtain photocatalyst and urges dry powder；
It counts in parts by weight, 40~50 parts of asphalt, 10~15 parts of atoleines is placed in stirred tank, it is heated to 90~
100 DEG C, with rotating speed 20~30min of insulated and stirred of 200~300r/min, then 10~15 parts of nitrile rubber are added into stirred tank
Powder continues 40~50min of stirring, obtains modified pitch, and gained modified pitch is put into oil bath pan, it is heated to 200~
220 DEG C, 10~15min is kept the temperature, 10~12 parts of dihydromethyl propionic acids, 8~10 parts of ethylene glycol, 15~20 parts of first are added to oil bath pan
Benzene, insulation reaction obtain carboxylated pitch；Count in parts by weight, by 30~40 parts of M-phthalic acids, 20~25 parts of neopentyl glycols,
5~10 parts of trimethylolpropanes, 1~3 part of Mono-n-butyltin mixing, are put into the four-hole boiling flask equipped with condensing unit, start
Blender is stirred with the rotating speed of 400~450r/min, is heated to 230~250 DEG C, under nitrogen protection, insulation reaction 2
10~15 parts of Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasics, 4~5 parts of carboxylated pitches are added after~3h, 2~3h of acidolysis reaction is cooled to room temperature,
Mix 20~30 parts of benzoyl peroxide methyl ethyl ketone, 10~12 parts of photocatalysts urge dry powder the reaction was continued 20~30min, obtain photocatalyst and urge
Dry Polyester Paint.
Count in parts by weight, to blender, reflux condensing tube, thermometer, dropping funel four-hole boiling flask in be added
50 parts of distilled water, 10 parts of dodecyl sodium sulfates, 4 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 200r/min, water-bath
70 DEG C are warming up to, after three-necked flasks are added in 40 parts of acrylic acid, 20 parts of methacrylic acids, the reaction was continued 10min obtains seed breast
Liquid；Count in parts by weight, into above-mentioned three-necked flask be added 20 parts of epoxidized soybean oils, then with dropping funel into four-hole boiling flask with
1 part of potassium peroxydisulfate is added dropwise in 3mL/min drop rates, and after being added dropwise, insulation reaction 30min continues to be heated to 90 DEG C, protect
Temperature reaction 45min, is cooled to 55 DEG C, and it is 6.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylic acid ester emulsion；
It is added 40mL absolute ethyl alcohols and 2g carbon nanotubes into ultrasonic disperse instrument, control supersonic frequency is 30kHz, ultrasonic disperse 4min,
Carbon nano tube suspension is obtained, carbon nano tube suspension is placed in the three-necked flask with blender and dropping funel, with drop
18mL butyl titanates are added into three-necked flask with the drop rate of 2mL/min for liquid funnel, while starting blender, with
The rotating speed of 200r/min starts stirring 10min and obtains mixed liquor；The second that 4mL mass fractions are 20% is added into above-mentioned mixed liquor
Acid solution, 20mL silicon dioxide gels stir 1h, obtain carbon nano-tube/titanic oxide colloidal sol, still aging 2 days, obtain dry molten
Dry colloidal sol is placed in the baking oven that set temperature is 60 DEG C by glue, and dry 10h obtains gel piece, gel piece is put into mortar and is ground
30min is ground, 200 mesh is crossed and sieves to obtain photocatalyst and urge dry powder；It counts in parts by weight, 40 parts of asphalt, 10 parts of atoleines is set
In stirred tank, 90 DEG C are heated to, with the rotating speed insulated and stirred 20min of 200r/min, then 10 parts are added into stirred tank
Nitrile rubber powder continues to stir 40min, obtains modified pitch, gained modified pitch is put into oil bath pan, is heated to 200
DEG C, 10min is kept the temperature, 10 parts of dihydromethyl propionic acids, 8 parts of ethylene glycol, 15 parts of toluene are added to oil bath pan, insulation reaction obtains carboxyl
Change pitch；It counts in parts by weight, by 30 parts of M-phthalic acids, 20 parts of neopentyl glycols, 5 parts of trimethylolpropanes, 1 part of monobutyl oxygen
Change tin mixing, be put into the four-hole boiling flask equipped with condensing unit, start blender, stirred with the rotating speed of 400r/min, heating rises
Temperature is to 230 DEG C, under nitrogen protection, 10 parts of Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasics, 4 parts of carboxylated pitches, acid is added after insulation reaction 2h
Solution reaction 2h, is cooled to room temperature, mixes 20 parts of benzoyl peroxide methyl ethyl ketone, and 10 parts of photocatalysts urge dry powder the reaction was continued 20min, obtain
Photocatalyst urges dry Polyester Paint.
Count in parts by weight, to blender, reflux condensing tube, thermometer, dropping funel four-hole boiling flask in be added
55 parts of distilled water, 12 parts of dodecyl sodium sulfates, 4 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 210r/min, water-bath
75 DEG C are warming up to, after three-necked flasks are added in 42 parts of acrylic acid, 25 parts of methacrylic acids, the reaction was continued 12min obtains seed
Lotion；It counts in parts by weight, 25 parts of epoxidized soybean oils is added into above-mentioned three-necked flask, then with dropping funel into four-hole boiling flask
2 parts of potassium peroxydisulfates are added dropwise with 4mL/min drop rates, after being added dropwise, insulation reaction 35min continues to be heated to 95 DEG C,
Insulation reaction 50min is cooled to 57 DEG C, and it is 6.5 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylate breast
Liquid；45mL absolute ethyl alcohols and 2g carbon nanotubes are added into ultrasonic disperse instrument, control supersonic frequency is 32kHz, ultrasonic disperse
5min obtains carbon nano tube suspension, and carbon nano tube suspension is placed in the three-necked flask with blender and dropping funel,
19mL butyl titanates are added into three-necked flask with the drop rate of 2mL/min with dropping funel, while starting blender, with
The rotating speed of 250r/min starts stirring 12min and obtains mixed liquor；The second that 4mL mass fractions are 20% is added into above-mentioned mixed liquor
Acid solution, 25mL silicon dioxide gels stir 1.5h, obtain carbon nano-tube/titanic oxide colloidal sol, still aging 2 days, done
Dry colloidal sol is placed in the baking oven that set temperature is 65 DEG C by colloidal sol, and dry 11h obtains gel piece, gel piece is put into mortar
32min is ground, 200 mesh is crossed and sieves to obtain photocatalyst and urge dry powder；It counts in parts by weight, by 45 parts of asphalt, 12 parts of atoleines,
It is placed in stirred tank, is heated to 95 DEG C, with the rotating speed insulated and stirred 25min of 250r/min, then 12 are added into stirred tank
Part nitrile rubber powder continues to stir 45min, obtains modified pitch, gained modified pitch is put into oil bath pan, is heated to
210 DEG C, 12min is kept the temperature, 11 parts of dihydromethyl propionic acids, 9 parts of ethylene glycol, 17 parts of toluene are added to oil bath pan, insulation reaction obtains
Carboxylated pitch；It counts in parts by weight, by 35 parts of M-phthalic acids, 22 parts of neopentyl glycols, 7 parts of trimethylolpropanes, 2 parts of only son
Base tin oxide mixes, and is put into the four-hole boiling flask equipped with condensing unit, starts blender, is stirred, is added with the rotating speed of 420r/min
Heat is warming up to 240 DEG C, under nitrogen protection, 12 parts of Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasics, 4 parts of carboxylated drips is added after insulation reaction 2.5h
Blueness, acidolysis reaction 2.5h are cooled to room temperature, mix 25 parts of benzoyl peroxide methyl ethyl ketone, 11 parts of photocatalysts urge dry powder, and the reaction was continued
25min obtains photocatalyst and urges dry Polyester Paint.
Count in parts by weight, to blender, reflux condensing tube, thermometer, dropping funel four-hole boiling flask in be added
60 parts of distilled water, 15 parts of dodecyl sodium sulfates, 5 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 220r/min, water-bath
80 DEG C are warming up to, after three-necked flasks are added in 45 parts of acrylic acid, 30 parts of methacrylic acids, the reaction was continued 15min obtains seed breast
Liquid；Count in parts by weight, into above-mentioned three-necked flask be added 30 parts of epoxidized soybean oils, then with dropping funel into four-hole boiling flask with
3 parts of potassium peroxydisulfates are added dropwise in 5mL/min drop rates, and after being added dropwise, insulation reaction 40min continues to be heated to 100 DEG C,
Insulation reaction 55min is cooled to 60 DEG C, and it is 7.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylate breast
Liquid；50mL absolute ethyl alcohols and 3g carbon nanotubes are added into ultrasonic disperse instrument, control supersonic frequency is 35kHz, ultrasonic disperse
6min obtains carbon nano tube suspension, and carbon nano tube suspension is placed in the three-necked flask with blender and dropping funel,
20mL butyl titanates are added into three-necked flask with the drop rate of 3mL/min with dropping funel, while starting blender, with
The rotating speed of 300r/min starts stirring 15min and obtains mixed liquor；The second that 5mL mass fractions are 20% is added into above-mentioned mixed liquor
Acid solution, 30mL silicon dioxide gels stir 2h, obtain carbon nano-tube/titanic oxide colloidal sol, still aging 3 days, done
Dry colloidal sol is placed in the baking oven that set temperature is 70 DEG C by colloidal sol, and dry 12h obtains gel piece, gel piece is put into mortar
35min is ground, 200 mesh is crossed and sieves to obtain photocatalyst and urge dry powder；It counts in parts by weight, by 50 parts of asphalt, 15 parts of atoleines,
It is placed in stirred tank, is heated to 100 DEG C, with the rotating speed insulated and stirred 30min of 300r/min, then 15 are added into stirred tank
Part nitrile rubber powder continues to stir 50min, obtains modified pitch, gained modified pitch is put into oil bath pan, is heated to
220 DEG C, 15min is kept the temperature, 12 parts of dihydromethyl propionic acids, 10 parts of ethylene glycol, 20 parts of toluene are added to oil bath pan, insulation reaction obtains
Carboxylated pitch；It counts in parts by weight, by 40 parts of M-phthalic acids, 25 parts of neopentyl glycols, 10 parts of trimethylolpropanes, 3 parts of lists
Butyl tin oxide mixes, and is put into the four-hole boiling flask equipped with condensing unit, starts blender, is stirred with the rotating speed of 450r/min,
250 DEG C are heated to, under nitrogen protection, 15 parts of Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasics, 5 parts of carboxylated drips are added after insulation reaction 3h
Blueness, acidolysis reaction 3h are cooled to room temperature, mix 30 parts of benzoyl peroxide methyl ethyl ketone, 12 parts of photocatalysts urge dry powder, and the reaction was continued
30min obtains photocatalyst and urges dry Polyester Paint.
Comparative example urges dry Polyester Paint to be touched as a comparison case to light produced by the present invention with the photocatalyst that Hebei company produces
Matchmaker urges the photocatalyst in dry Polyester Paint and comparative example that dry Polyester Paint is urged to carry out performance detection, and testing result is as shown in table 1：
Test method：
Adhesive force test is detected by GB9286 scratchs；
Yellowness index test method is tested by the saying of xanthochromia series Δ Yi, is divided by yellowness index：
0 grade：Without discoloration, Δ Yi≤1.5；1 grade：Very light discolouration, 1.6 ＜ Δs Yi≤3.0；2 grades：Light discolouration, 3.1
＜ Δs Yi≤6.0；3 grades：Apparent discoloration, 6.1 ＜ Δs Yi≤9.0；4 grades：Larger discoloration, 9.1 ＜ Δs Yi≤12.0；
5 grades：Serious discoloration, 12.0 ＜ Δs Yi；
Impact resistance test method：It takes Polyester Paint in example 1~3 and comparative example to be coated on film for use, paint film is put down upward
It is placed on anvil, the weight for preparing a fixed mass is for use, and weight borrows a certain height that control device is fixed on slide cartridge, pressing
Control knob, weight are freely fallen on paint film, lift weight, and each paint film respectively repeats 3 height, and record weight falls within sample
On height；
1 Polyester Paint performance measurement result of table
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Adhesive force（Grade） | 0 | 0 | 0 | 2 |
| Anti-ultraviolet ageing performance yellowness index（ΔYi） | 0.4 | 0.3 | 0.2 | 3.5 |
| 15cm height | It is unchanged | It is unchanged | It is unchanged | Slight slight crack |
| 30cm height | It is unchanged | It is unchanged | It is unchanged | Apparent embrittlement |
| 45cm height | Slight deformation | Slight slight crack | It is unchanged | Obviously split |
Urge dry Polyester Paint adhesive force good according to the photocatalyst produced by the present invention of data among the above, anti-ultraviolet ageing performance is good,
Yellowness index only 0.2 Δ Yi, is not easy xanthochromia, good impact resistance, flexibility is good, and when stress is not easy embrittlement, and environment friendly is good, tool
Have broad application prospects.
Claims (7)
1. a kind of photocatalyst urges the preparation method of dry Polyester Paint, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, to blender, reflux condensing tube, thermometer, dropping funel four-hole boiling flask in be added 50
~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates start blender with 200~220r/min
Rotating speed stirring, warming-in-water after three-necked flasks are added in 40~45 parts of acrylic acid, 20~30 parts of methacrylic acids, continues anti-
It should obtain seed emulsion；
（2）It counts in parts by weight, 20~30 parts of epoxidized soybean oils is added into above-mentioned three-necked flask, then with dropping funel to four mouthfuls
1~3 part of potassium peroxydisulfate is added dropwise in drop rate in flask, and after being added dropwise, insulation reaction continues heat temperature raising, after insulation reaction
Cooling adjusts pH with ammonium hydroxide, and discharging obtains acrylic acid ester emulsion；
（3）40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and 2~3g carbon nanotubes, ultrasonic disperse obtain carbon nanotube
Carbon nano tube suspension is placed in the three-necked flask with blender and dropping funel by suspension, and speed is added dropwise with dropping funel
18~20mL butyl titanates are added into three-necked flask for rate, while starting blender, are started with the rotating speed of 200~300r/min
10~15min of stirring obtains mixed liquor；
（4）4~5mL acetic acid solutions are added into above-mentioned mixed liquor, 20~30mL silicon dioxide gels stir 1~2h, obtain
Carbon nano-tube/titanic oxide colloidal sol, it is still aging to obtain dry colloidal sol, dry colloidal sol is placed in baking oven, it is dry, gel piece is obtained,
Gel piece is put into mortar and is ground, sieving obtains photocatalyst and urges dry powder；
（5）It counts in parts by weight, 40~50 parts of asphalt, 10~15 parts of atoleines is placed in stirred tank, heating rises
Temperature, insulated and stirred, then 10~15 parts of nitrile rubber powders are added into stirred tank, continue to stir, obtain modified pitch, gained is modified
Pitch is put into oil bath pan, heat temperature raising, heat preservation, and 10~12 parts of dihydromethyl propionic acids, 8~10 parts of second two are added to oil bath pan
Alcohol, 15~20 parts of toluene, insulation reaction obtain carboxylated pitch；
（6）It counts in parts by weight, by 30~40 parts of M-phthalic acids, 20~25 parts of neopentyl glycols, 5~10 parts of trihydroxy methyls third
Alkane, the mixing of 1~3 part of Mono-n-butyltin, are put into the four-hole boiling flask equipped with condensing unit, start blender, with 400~
The rotating speed of 450r/min stirs, heat temperature raising, under nitrogen protection, 10~15 parts of Isosorbide-5-Nitraes-hexamethylene diformazan is added after insulation reaction
Acid, 4~5 parts of carboxylated pitches, acidolysis reaction are cooled to room temperature, mix 20~30 parts of benzoyl peroxide methyl ethyl ketone, 10~12 parts of light
Catalyst urges dry powder, and the reaction was continued, obtains photocatalyst and urges dry Polyester Paint.
2. a kind of photocatalyst according to claim 1 urges the preparation method of dry Polyester Paint, it is characterised in that：Step（1）Institute
Temperature is 70~80 DEG C after the warming-in-water stated, and reacts 10~15min.
3. a kind of photocatalyst according to claim 1 urges the preparation method of dry Polyester Paint, it is characterised in that：Step（2）Institute
The dropping funel drop rate stated is 3~5mL/min, and the insulation reaction time is 30~40min, and temperature is after continuing heat temperature raising
90~100 DEG C, the insulation reaction time is 45~55min, and temperature is 55~60 DEG C after cooling, the mass fraction 20% of ammonium hydroxide, ammonium hydroxide
It is 6.0~7.0 to adjust pH.
4. a kind of photocatalyst according to claim 1 urges the preparation method of dry Polyester Paint, it is characterised in that：Step（3）Institute
The control supersonic frequency stated is 30~35kHz, and the ultrasonic disperse time is 4~6min, 2~3mL/min of dropping funel drop rate.
5. a kind of photocatalyst according to claim 1 urges the preparation method of dry Polyester Paint, it is characterised in that：Step（4）Institute
The mass fraction for the acetic acid solution stated is 20%, and the still aging time is 2~3 days, and baking oven set temperature is 60~70 DEG C, dry
Time is 10~12h, and milling time is 30~35min, and be sieved specification is 200 mesh.
6. a kind of photocatalyst according to claim 1 urges the preparation method of dry Polyester Paint, it is characterised in that：Step（5）Institute
Temperature is 90~100 DEG C after the heat temperature raising stated, and temperature is 200~220 DEG C after oil bath pan heat temperature raising, soaking time is 10~
15min。
7. a kind of photocatalyst according to claim 1 urges the preparation method of dry Polyester Paint, it is characterised in that：Step（6）Institute
Temperature is 230~250 DEG C after the four-hole boiling flask heat temperature raising stated, and the insulation reaction time is 2~3h under nitrogen protection, and acidolysis is anti-
It is 2~3h between seasonable, continues the reaction time after being cooled to room temperature as 20~30min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109135600A (en) * | 2018-09-08 | 2019-01-04 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of the thermally conductive foam tape of heat oxygen aging resistance |
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