CN106497373A - A kind of preparation method of aqueous polyurethane fluorocarbon coating - Google Patents
A kind of preparation method of aqueous polyurethane fluorocarbon coating Download PDFInfo
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
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- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a kind of preparation method of aqueous polyurethane fluorocarbon coating, belongs to technical field of coatings.The invention provides a kind of preparation method of aqueous polyurethane fluorocarbon coating, the present invention is with trimethylolpropane, N methyl diethanolamines, plus isophorone diisocyanate etc. is raw material, prepare water-based hydroxyl terminated cationic polyurethane, and it is configured to emulsion, again with styrene as monomer, nano-silica surface is coated on by polyreaction, prepared modified manometer silicon dioxide, finally by water-based hydroxyl terminated cationic polyurethane emulsion, modified manometer silicon dioxide, after the ball milling mixings such as FEVE fluorocarbon resins, disperseed with high-speed shearing machine again, it is configured to aqueous polyurethane fluorocarbon coating, the aqueous polyurethane fluorocarbon coating energy-saving safe that the present invention is prepared is pollution-free, impervious, dirt-resistant thermostability, corrosion resistance, chemical-resistant is good.
Description
Technical field
The invention discloses a kind of preparation method of aqueous polyurethane fluorocarbon coating, belongs to technical field of coatings.
Background technology
Traditional oil paint is often inflammable and explosive, the aspect such as uses all there is larger safety in production, transport, storage
Hidden danger, and oil paint is mostly containing the toxic solvent such as stupid, larger to harm, also bring more serious environmental issue.
With the enhancing of people's environmental consciousness, volatile organic matter(VOC)Burst size is low, adhesive force is strong, good to material surface adaptability
Water paint, gradually enter into the sight line of people and capture rapidly Coating Market in recent years, water paint do not contain benzene kind solvent
And there is no the environmental protection that brought of inflammable and explosive property and safety.Oil paint is compared to, water paint is acidproof, resistance to
The performances such as water, salt spray resistance are more excellent, and coating be easy to construct, spray, dip-coating or roller coat all without drawback, and apply
Coating adhesion strong, difficult for drop-off, aging.
Existing Chinese patent literature CN1109726 and CN1613931 individually disclose 2 kinds of water soluble paints.But mesh
On front market, the baking film-forming temperature of water soluble paint is actually universal all in 180 degree or so, and higher temperature requirement is caused
The raising of production cost, and some coated periods, as some plastics, metallic aluminium, zinc and some alloys etc. high
At a temperature of be easily deformed losing shape, and have impact on the application of water soluble paint, meanwhile, some water soluble paints on the market
In due to the content of defoamer higher, easily cause coating surface when foam is abolished and form shrinkage cavity or fried speckle so that apply
The levelling effect of material is not good enough.Additionally, there is some water soluble paints also to there is bad adhesive force, aging resistance, chemical resistance, anti-
The problem of ultraviolet effect difference, causes the paint film for coating easily to come off after a period of time has passed, eclipsed or bleeding etc..Due to
Water soluble paint is with water as basic solvent, even adding various surfactants, emulsifying agent to carry in formulation for coating material
The compatibility and water solublity between high each composition, but traditional preparation technology is still difficult to synergistically melt all of dispensing
It is combined and does not affect respective efficiency.The baking film-forming temperature of water soluble paint is actually universal all 180 in the market
More than degree, higher temperature requirement causes the raising of production cost, and construction technology can not implement wet on wet technique so that spray
The efficiency for applying production is low, high energy consumption, and the coating bottom surface oil when glass, pottery and hardware products are electroplated all is that oiliness is applied
Material, does not meet the scientific development trend of environmental protection.Therefore, how to overcome in water soluble paint formula and preparation technology and generally deposit
Drawbacks described above become water soluble paint exploitation trend.
Content of the invention
Present invention mainly solves technical problem:Bad, anti-ageing for the not good enough adhesive force of existing water paint levelling effect
Change, chemical resistance, the problem of uvioresistant effect difference, the invention provides a kind of preparation of aqueous polyurethane fluorocarbon coating
Method, the present invention prepare water with trimethylolpropane, N methyldiethanol amine, plus isophorone diisocyanate etc. for raw material
Cardinal extremity hydroxyl cation polyurethane, and emulsion is configured to, then with styrene as monomer, nanometer is coated on by polyreaction
Silica surface, is obtained modified manometer silicon dioxide, finally by water-based hydroxyl terminated cationic polyurethane emulsion, modified Nano two
After the ball milling mixings such as silicon oxide, FEVE fluorocarbon resins, then disperseed with high-speed shearing machine, be configured to aqueous polyurethane fluorocarbon coating,
The aqueous polyurethane fluorocarbon coating energy-saving safe that the present invention is prepared is pollution-free, impermeability, dirt-resistant thermostability, corrosion-resistant
Property, chemical-resistant are good.
The present invention is a kind of preparation method of aqueous polyurethane fluorocarbon coating, it is characterised in that specifically preparation process is:
(1)1.5~1.8g trimethylolpropanes are weighed, with 18~20mL N methyldiethanol amines, is loaded in reactor, heating
To 100~105 DEG C, and 1~2h of keeping temperature, 40~50 DEG C are subsequently cooled to, then with the different Fo Er of 1mL/min 18~20mL of Deca
Ketone diisocyanate, is added 0.1~0.2mL dibutyl tin laurates after completion of dropping, and is stirred with 300~400r/min
1~2h is mixed, reactant liquor is obtained;
(2)To in above-mentioned reactant liquor, add glacial acetic acid to reactant liquor pH in neutrality, stand 30~40min, obtain water base terminal hydroxy group sun
Ion polyurethane, subsequently proceeds to water-based hydroxyl terminated cationic polyurethane in 120~150mL deionized waters, and with 500~
600r/min stirs 20~30min, obtains water-based hydroxyl terminated cationic polyurethane emulsion, standby;
(3)Weigh 3~6g nano silicons, add in 11~22mL styrene, with 300~400r/min stirrings 10~
15min, adds 0.75~1.50g Silane coupling reagent KH-570s, and disperses 10~15min with 200W ultrasonic echographies, subsequently
0.5~1.0g dodecyl sodium sulfates, 0.5~1.0g alkylphenol polyoxyethylene, 100~120mL deionized waters is added to continue
After 10~15min of stirring, load in high-shear homogenizer and disperse 5~8min, obtain mixed emulsion;
(4)Above-mentioned mixed emulsion is loaded in reactor, 50~60 DEG C is warming up to, and is added 0.01~0.02g potassium peroxydisulfates,
Under nitrogen atmosphere, 70~75 DEG C are continuously heating to, are incubated 4~5h, add 80~100mL dehydrated alcohol, stand 1~2h, with
After filter, and wash filtering residue 3~5 times with mass fraction for 50% ethanol solution, then filtering residue be placed in vacuum drying oven, 60
15~20h is dried at~70 DEG C, modified manometer silicon dioxide is obtained;
(5)Count by weight, weigh 20~30 parts of FEVE fluorocarbon resins, 30~40 parts of steps(2)The water base terminal hydroxy group for preparing
Cation polyurethane emulsion, 5~8 parts of above-mentioned modified manometer silicon dioxides, 1~2 part of dispersant EFA-1010,2~5 parts of polytetrafluoros
Ethylene, loads in ball mill, with 300~400r/min, 20~30min of ball milling, is subsequently added in high-speed shearing machine, with 8000~
12000r/min disperses 10~15min, and is filtered with 200 mesh filter screens, obtains aqueous polyurethane fluorocarbon coating.
The application process of the present invention:From tinplate as base plate, wine is used with sand papering tinplate to rustless first
Smart cotton rub is wiped, and is dried naturally, will in aqueous polyurethane fluorocarbon coating add 5~25% clear water release dilute stir, process
Brushing paint on tinplate afterwards, in the environment of being placed horizontally at 20~30 DEG C of temperature, dries 5~7h, now tinplate
Upper appearance of film is smooth, pliability, good impact resistance.
The invention has the beneficial effects as follows:
(1)Aqueous polyurethane fluorocarbon coating prepared by the present invention, makees solvent with water, zero or low VOC, production safety, power-save operation
Convenient, it is not detrimental to health, environmentally safe;
(2)Aqueous polyurethane fluorocarbon coating prepared by the present invention, impervious good, there are superior barrier propterty, acidproof, salt, sea water
Deng;
(3)Aqueous polyurethane fluorocarbon coating prepared by the present invention, adhesive force are good, and soft durometer scalable meets the need of different clients
Ask, dirt-resistant, hydrophobicity, weather resisteant colour retention and thermostability, corrosion resistance, chemical-resistant are good.
Specific embodiment
1.5~1.8g trimethylolpropanes are weighed, with 18~20mL N methyldiethanol amines, is loaded in reactor, heating
To 100~105 DEG C, and 1~2h of keeping temperature, 40~50 DEG C are subsequently cooled to, then with the different Fo Er of 1mL/min 18~20mL of Deca
Ketone diisocyanate, is added 0.1~0.2mL dibutyl tin laurates after completion of dropping, and is stirred with 300~400r/min
1~2h is mixed, reactant liquor is obtained, in above-mentioned reactant liquor, is added glacial acetic acid to reactant liquor pH in neutrality, is stood 30~40min, obtain water
Cardinal extremity hydroxyl cation polyurethane, subsequently proceeds to water-based hydroxyl terminated cationic polyurethane in 120~150mL deionized waters, and
20~30min is stirred with 500~600r/min, water-based hydroxyl terminated cationic polyurethane emulsion is obtained, standby, weigh 3~6g nanometers
Silicon dioxide, adds in 11~22mL styrene, stirs 10~15min with 300~400r/min, add 0.75~1.50g
Silane coupling reagent KH-570, and 10~15min is disperseed with 200W ultrasonic echographies, it is subsequently added 0.5~1.0g dodecyl sulphurs
Sour sodium, 0.5~1.0g alkylphenol polyoxyethylene, 100~120mL deionized waters, after continuing 10~15min of stirring, load high
Disperse 5~8min in fast homogenizer, obtain mixed emulsion, above-mentioned mixed emulsion is loaded in reactor, 50~60 DEG C are warming up to, and
0.01~0.02g potassium peroxydisulfates are added, under nitrogen atmosphere, 70~75 DEG C is continuously heating to, 4~5h is incubated, add 80~
100mL dehydrated alcohol, stands 1~2h, subsequently filters, and washs filtering residue 3~5 times, then general with mass fraction for 50% ethanol solution
Filtering residue is placed in vacuum drying oven, dries 15~20h, obtain modified manometer silicon dioxide, count by weight at 60~70 DEG C,
Weigh 20~30 parts of FEVE fluorocarbon resins, 30~40 parts of steps(2)The water-based hydroxyl terminated cationic polyurethane emulsion of preparation, 5~8
The above-mentioned modified manometer silicon dioxide of part, 1~2 part of dispersant EFA-1010,2~5 parts of politef load in ball mill, with
300~400r/min, 20~30min of ball milling, are subsequently added in high-speed shearing machine, with 8000~12000r/min dispersion 10~
15min, and filtered with 200 mesh filter screens, obtain aqueous polyurethane fluorocarbon coating.
Example 1
1.5g trimethylolpropanes are weighed, with 18mL N methyldiethanol amines, is loaded in reactor, is heated to 100 DEG C, and protects
Temperature 1h is held, 40 DEG C are subsequently cooled to, then with 1mL/min Deca 18mL isophorone diisocyanate, after completion of dropping again
0.1mL dibutyl tin laurates being added, and 1h being stirred with 300r/min, obtain reactant liquor, ice vinegar is added in above-mentioned reactant liquor
Acid in neutrality, stands 30min, obtains water-based hydroxyl terminated cationic polyurethane, subsequently by water base terminal hydroxy group cation to reactant liquor pH
Polyurethane is proceeded in 120mL deionized waters, and stirs 20min with 500r/min, obtains water-based hydroxyl terminated cationic polyurethane emulsion,
Standby, 3g nano silicons are weighed, is added in 11mL styrene, 10min is stirred with 300r/min, 0.75g silane is added
Coupling agent kh-570, and 10min is disperseed with 200W ultrasonic echographies, it is subsequently added 0.5g dodecyl sodium sulfates, 0.5g alkyl
Phenol polyethenoxy ether, 100mL deionized waters, after continuing stirring 10min, load in high-shear homogenizer and disperse 5min, must mix breast
Liquid, above-mentioned mixed emulsion is loaded in reactor, 50 DEG C is warming up to, and is added 0.01g potassium peroxydisulfates, under nitrogen atmosphere, after
Continue and be warming up to 70 DEG C, be incubated 4h, add 80mL dehydrated alcohol, stand 1h, subsequently filter, and be 50% ethanol with mass fraction
Solution washing filtering residue 3 times, then filtering residue is placed in vacuum drying oven, 15h is dried at 60 DEG C, obtain modified manometer silicon dioxide,
Count by weight, weigh 20 parts of FEVE fluorocarbon resins, 30 parts of steps(2)The water-based hydroxyl terminated cationic polyurethane breast of preparation
Liquid, 5 parts of above-mentioned modified manometer silicon dioxides, 1 part of dispersant EFA-1010,2 parts of politef load in ball mill, with
300r/min ball milling 20min, are subsequently added in high-speed shearing machine, disperse 10min with 8000r/min, and with 200 mesh filter screen mistakes
Filter, obtains aqueous polyurethane fluorocarbon coating.
The application process of the present invention:From tinplate as base plate, wine is used with sand papering tinplate to rustless first
Smart cotton rub is wiped, and is dried naturally, will in aqueous polyurethane fluorocarbon coating add 5% clear water release dilute stir, after treatment
Brushing paint on tinplate, in the environment of being placed horizontally at 20 DEG C of temperature, dries 5h, and now on tinplate, appearance of film is put down
Whole, pliability, good impact resistance.
Example 2
1.65g trimethylolpropanes are weighed, with 19mL N methyldiethanol amines, is loaded in reactor, is heated to 102.5 DEG C, and
Keeping temperature 1.5h, is subsequently cooled to 45 DEG C, then with 1mL/min Deca 19mL isophorone diisocyanate, treats completion of dropping
After add 0.15mL dibutyl tin laurates, and 1.5h is stirred with 350r/min, obtains reactant liquor, in above-mentioned reactant liquor plus
Enter glacial acetic acid to reactant liquor pH in neutrality, stand 35min, obtain water-based hydroxyl terminated cationic polyurethane, subsequently by water base terminal hydroxy group
Cation polyurethane is proceeded in 135mL deionized waters, and stirs 25min with 550r/min, obtains water base terminal hydroxy group polyurethane/cationic
Ester emulsion, standby, 4.5g nano silicons are weighed, is added in 16.5mL styrene, 12.5min is stirred with 350r/min, then
1.125g Silane coupling reagent KH-570s are added, and 12.5min is disperseed with 200W ultrasonic echographies, be subsequently added 0.75g dodecanes
Base sodium sulfonate, 0.75g alkylphenol polyoxyethylene, 110mL deionized waters, after continuing stirring 12.5min, load high-shear homogenizer
Middle dispersion 6.5min, obtains mixed emulsion, above-mentioned mixed emulsion is loaded in reactor, 55 DEG C is warming up to, and is added 0.015g mistakes
Potassium sulfate, under nitrogen atmosphere, is continuously heating to 72.5 DEG C, is incubated 4.5h, adds 90mL dehydrated alcohol, stands 1.5h, with
After filter, and wash filtering residue 4 times with mass fraction for 50% ethanol solution, then filtering residue be placed in vacuum drying oven, at 65 DEG C
17.5h is dried, modified manometer silicon dioxide is obtained, is counted by weight, weigh 25 parts of FEVE fluorocarbon resins, 35 parts of steps(2)System
Standby water-based hydroxyl terminated cationic polyurethane emulsion, 6 parts of above-mentioned modified manometer silicon dioxides, 1 part of dispersant EFA-1010,3 parts
Politef, loads in ball mill, with 350r/min ball milling 25min, is subsequently added in high-speed shearing machine, with 10000r/min
Dispersion 12.5min, and filtered with 200 mesh filter screens, obtain aqueous polyurethane fluorocarbon coating.
The application process of the present invention:From tinplate as sample base plate, first with sand papering tinplate to rustless,
With alcohol swab wipe, dry naturally, will in aqueous polyurethane fluorocarbon coating add 15% clear water release dilute stir, process
Brushing paint on tinplate afterwards, in the environment of being placed horizontally at 25 DEG C of temperature, dries 6h, now on tinplate outside film
See smooth, pliability, good impact resistance.
Example three
1.8g trimethylolpropanes are weighed, with 20mL N methyldiethanol amines, is loaded in reactor, is heated to 105 DEG C, and protects
Temperature 2h is held, 50 DEG C are subsequently cooled to, then with 1mL/min Deca 20mL isophorone diisocyanate, after completion of dropping again
0.2mL dibutyl tin laurates being added, and 2h being stirred with 400r/min, obtain reactant liquor, ice vinegar is added in above-mentioned reactant liquor
Acid in neutrality, stands 40min, obtains water-based hydroxyl terminated cationic polyurethane, subsequently by water base terminal hydroxy group cation to reactant liquor pH
Polyurethane is proceeded in 150mL deionized waters, and stirs 30min with 600r/min, obtains water-based hydroxyl terminated cationic polyurethane emulsion,
Standby, 6g nano silicons are weighed, is added in 22mL styrene, 15min is stirred with 400r/min, 1.50g silane is added
Coupling agent kh-570, and 15min is disperseed with 200W ultrasonic echographies, it is subsequently added 1.0g dodecyl sodium sulfates, 1.0g alkyl
Phenol polyethenoxy ether, 120mL deionized waters, after continuing stirring 15min, load in high-shear homogenizer and disperse 8min, must mix breast
Liquid, above-mentioned mixed emulsion is loaded in reactor, 60 DEG C is warming up to, and is added 0.02g potassium peroxydisulfates, under nitrogen atmosphere, after
Continue and be warming up to 75 DEG C, be incubated 5h, add 100mL dehydrated alcohol, stand 2h, subsequently filter, and be 50% ethanol with mass fraction
Solution washing filtering residue 5 times, then filtering residue is placed in vacuum drying oven, 20h is dried at 70 DEG C, obtain modified manometer silicon dioxide,
Count by weight, weigh 30 parts of FEVE fluorocarbon resins, 40 parts of steps(2)The water-based hydroxyl terminated cationic polyurethane breast of preparation
Liquid, 8 parts of above-mentioned modified manometer silicon dioxides, 2 parts of dispersant EFA-1010,5 parts of politef load in ball mill, with
400r/min ball milling 30min, are subsequently added in high-speed shearing machine, disperse 15min with 12000r/min, and with 200 mesh filter screen mistakes
Filter, obtains aqueous polyurethane fluorocarbon coating.
The application process of the present invention:From tinplate as sample base plate, first with sand papering tinplate to rustless,
With alcohol swab wipe, dry naturally, will in aqueous polyurethane fluorocarbon coating add 25% clear water release dilute stir, process
Brushing paint on tinplate afterwards, in the environment of being placed horizontally at 30 DEG C of temperature, dries 7h, now on tinplate outside film
See smooth, pliability, good impact resistance.
Claims (1)
1. a kind of preparation method of aqueous polyurethane fluorocarbon coating, it is characterised in that concrete preparation process is:
(1)1.5 ~ 1.8g trimethylolpropanes are weighed, with 18 ~ 20mL N methyldiethanol amines, is loaded in reactor, is heated to
100 ~ 105 DEG C, and 1 ~ 2h of keeping temperature, 40 ~ 50 DEG C are subsequently cooled to, then different with 1mL/min 18 ~ 20mL of Deca isophorones two
Cyanate, adds 0.1 ~ 0.2mL dibutyl tin laurates after completion of dropping, and stirs 1 ~ 2h with 300 ~ 400r/min,
Obtain reactant liquor;
(2)To in above-mentioned reactant liquor, add glacial acetic acid to reactant liquor pH in neutrality, stand 30 ~ 40min, obtain water base terminal hydroxy group sun from
Sub- polyurethane, subsequently proceeds to water-based hydroxyl terminated cationic polyurethane in 120 ~ 150mL deionized waters, and with 500 ~ 600r/min
20 ~ 30min of stirring, obtains water-based hydroxyl terminated cationic polyurethane emulsion, standby;
(3)3 ~ 6g nano silicons are weighed, is added in 11 ~ 22mL styrene, 10 ~ 15min is stirred with 300 ~ 400r/min, then
0.75 ~ 1.50g Silane coupling reagent KH-570s are added, and 10 ~ 15min is disperseed with 200W ultrasonic echographies, it is subsequently added 0.5 ~
1.0g dodecyl sodium sulfates, 0.5 ~ 1.0g alkylphenol polyoxyethylene, 100 ~ 120mL deionized waters, continue stirring 10 ~
After 15min, load in high-shear homogenizer and disperse 5 ~ 8min, obtain mixed emulsion;
(4)Above-mentioned mixed emulsion is loaded in reactor, 50 ~ 60 DEG C is warming up to, and is added 0.01 ~ 0.02g potassium peroxydisulfates, in nitrogen
Under atmosphere is enclosed, 70 ~ 75 DEG C are continuously heating to, are incubated 4 ~ 5h, add 80 ~ 100mL dehydrated alcohol, stood 1 ~ 2h, subsequently filter,
And filtering residue 3 ~ 5 times is washed with mass fraction for 50% ethanol solution, then filtering residue is placed in vacuum drying oven, do at 60 ~ 70 DEG C
Dry 15 ~ 20h, obtains modified manometer silicon dioxide;
(5)Count by weight, weigh 20 ~ 30 parts of FEVE fluorocarbon resins, 30 ~ 40 parts of steps(2)The water base terminal hydroxy group sun for preparing
Ion polyaminoester emulsion, 5 ~ 8 parts of above-mentioned modified manometer silicon dioxides, 1 ~ 2 part of dispersant EFA-1010,2 ~ 5 parts of politef,
Load in ball mill, with 300 ~ 400r/min, 20 ~ 30min of ball milling, be subsequently added in high-speed shearing machine, with 8000 ~ 12000r/
Min disperses 10 ~ 15min, and is filtered with 200 mesh filter screens, obtains aqueous polyurethane fluorocarbon coating.
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