CN109554096A - A kind of preparation method of light-resistant waterborne polyurethane coating - Google Patents
A kind of preparation method of light-resistant waterborne polyurethane coating Download PDFInfo
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- CN109554096A CN109554096A CN201811461308.0A CN201811461308A CN109554096A CN 109554096 A CN109554096 A CN 109554096A CN 201811461308 A CN201811461308 A CN 201811461308A CN 109554096 A CN109554096 A CN 109554096A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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Abstract
The invention discloses a kind of preparation methods of light-resistant waterborne polyurethane coating, equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, dihydric alcohol 14.8g, isocyanates 53.2g are mixed, under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g, 1 ~ 3h is reacted at 75 ~ 80 DEG C, obtains base polyurethane prepolymer for use as A；Dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 ~ 80 DEG C of reaction 2.5h, triethylamine 9.4g is added and carries out 30 ~ 60min of neutralization reaction, add water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g and crosslinking agent 0.02g is added, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH is 7 ~ 8, obtains light-resistant waterborne polyurethane coating, and resulting materials have very strong light resistance.
Description
Technical field
The invention belongs to aqueous polyurethane coating fields, and in particular to a kind of preparation side of light-resistant waterborne polyurethane coating
Method.
Background technique
Polyurethane (PU) material due to having high intensity, tear-proof, the characteristics such as wear-resisting and elasticity is good, with cream
The forms such as liquid, resin, elastomer be widely used in transport, household electrical appliances, machinery, building, light textile, shoemaking, sports goods and place,
The fields such as agricultural, national defence are a kind of multi-functional polymer materials.Polyurethane is according to the type difference of isocyanate material point
For aromatic urethane and aliphatic polyurethane.Aliphatic polyurethane properties of product are relatively stable, the performances such as intensity, durability
All preferably, but price is relatively high;And the performance of aromatic urethane product and the performance of aliphatic polyurethane product are equal to
Beauty, and it is cheap, unique defect is that its portioned product performance is unstable, and especially white or light coloured fabrics are ultraviolet
Under the action of line, the ammonia ester bond in structure easily decomposes, aoxidizes generation quinones chromophoric group, the methylene being connected with phenyl ring easily quilt
Oxidation brings it about xanthochromia.All use cost performance high due to most of PU resins methyl diphenylene diisocyanate (
) etc. MDI aromatic isocyanates are as raw material, and since phenyl ring is directly connect with isocyanate groups in MDI, on phenyl ring
Big pi bond and neighbouring-NCO formed and be conjugated, so, using MDI as PU resin made of raw material, in light, heat, oxygen
Under environment, especially polyurethane is easy to cause polyurethane chain fracture, crosslinking, drop after absorbing 290~400 nm ultraviolet lights
Solution generates chromophoric group, causes the mechanical property and anti-yellowing property decline of polyurethane product.Therefore, aromatic urethane is solved
Xanthochromia problem it is significant to the development of Polyurethane Industry.
After the xanthochromia of polyurethane refers to that it reuses a period of time, the sharp process turned yellow of pure white paint film, one
As xanthochromia speed it is very slow, only reaching certain time can just display.Polyurethane why xanthochromia, it is main or high temperature,
Oxidation reaction occurs for film aging under the influence of 3 aspects such as illumination, reaction.After polyurethane oxidation, phenyl ring in coating with
Carbamate conjugated structure sequence is resequenced, and the quinoid structure with chromophoric group is formed.Illumination factor is paint film xanthochromia
Reaction provides energy, causes coating gradually degradation with aging, unsaturated bond is the fundamental cause of coating xanthochromia, the painting containing unsaturated bond
Material just has the possibility of discoloration, and the speed of last paint film xanthochromia again influences the absorption intensity of ultraviolet light by coating pigments and fillers.
The 201711369135.5 disclosure of the invention polyurethane coating and preparation method thereof of fire-retardant, light resistance and low VOC,
With blender, condenser pipe, thermometer 250ml there-necked flask in be added triethylene tetramine 0.22g, polytetrahydrofuran ether glycol
70g and hexamethylene diisocyanate 15g, reacts 2h at 80 DEG C, obtains base polyurethane prepolymer for use as A；It is added into performed polymer A
0.62g acetamide and 8.2g methyl ethyl ketone, react 3.5h under the conditions of 75 DEG C, be added 2g step (1) preparation modification manganese hypophosphite,
80 DEG C of reaction temperature, reaction time 2h, tri- second of 7.1g is added in 4g4- Carboxybenzeneboronic acid and diethylene triamine pentamethylene phosphonic 2.5g
Amine carries out neutralization reaction 60min, and addition vitamin C 0.9g, water 70g are stirred emulsification, obtain fire-retardant, light resistance and low VOC
Polyurethane coating, it is the polyurethane coating environmental protection of prepared fire-retardant, light resistance and low VOC, cheap, be widely used in wall
Body, furniture, ironware surface, as plastics, glass, papermaking, weaving adhesive.
Summary of the invention
The invention discloses the preparation method of light-resistant waterborne polyurethane coating, traditional isocyanates with phenyl ring exists
The defect turned to be yellow under long-term sunlight, the present invention use 2,2'- bipyridyl, phenyl-phosphonic acid, anhydrous cupric sulfate, sodium molybdate, object
The prepared inhibitor to light with very high inhibition effect of matter A and substance B, reduce phenyl ring and are oxidized to quinoid structure, object
The combination of sodium molybdate, 2,2'- bipyridyl is respectively increased in matter A and substance B, greatly improves the resistance to light effect of light inhibitor.
A kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, substance A 0.0161g and substance B 0.0012g, are placed in the closed container of 50mL, add
The distilled water of 15g is stirred to react 30 ~ 60min, adjusts pH to 5, is stirred to react 15 ~ 21h at 85 ~ 95 DEG C, is cooled at 50 DEG C certainly
So cooling, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by dihydric alcohol 14.8g, isocyanates
53.2g mixing under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g, 1 ~ 3h is reacted at 75 ~ 80 DEG C, is gathered
Urethane performed polymer A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 ~ 0 DEG C of reaction 2.5h, triethylamine 9.4g is added
30 ~ 60min of neutralization reaction is carried out, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g is added
With crosslinking agent 0.02g, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain aqueous polyurethane coating.
Substance A is 2- methoxyl group -4- methylphenol, 2,6- syringol, 3,3- dimethacrylate, chloroacetic acid
Any one；Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g at 50 ~ 60 DEG C
It is stirred to react 1 ~ 2h, add 5ml water and adjusts pH to 4, the reaction was continued 30min obtains substance B；The dihydric alcohol is poly- tetrahydro furan
Mutter ether glycol, polycarbonate glycol, 1,4- butanediol any one；The number-average molecular weight of the polytetrahydrofuran ether glycol
For any one of 1000,1800,2000；The number-average molecular weight of the polycarbonate glycol be 1000 and 2000 it is any one
Kind；The isocyanates is any one of toluene di-isocyanate(TDI) (TDI), '-diphenylmethane diisocyanate (MDI)；The friendship
Connection agent is any one of diethylenetriamine, tetraethylenepentamine, dimethylamine propylamine.
Present invention has an advantage that
(1) present invention is using the prepared of 2,2'- bipyridyl, phenyl-phosphonic acid, anhydrous cupric sulfate, sodium molybdate, substance A and substance B
The inhibitor to light with very high inhibition effect, reduction phenyl ring is oxidized to quinoid structure, and substance A and substance B are respectively increased
The combination of sodium molybdate, 2,2'- bipyridyl greatly improves the resistance to light effect of light inhibitor.
(2) advantage of the invention is that mainly solving the xanthochromia technical problem of MDI and TDI containing phenyl ring.
(3) advantage that there is light inhibitor of the invention the reaction time to shorten.
Specific embodiment
Embodiment 1
A kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, 2- methoxyl group -4- methylphenol 0.0161g and substance B 0.0012g, are placed in the closed of 50mL
In container, the distilled water of 15g is added, is stirred to react 30min, pH to 5 is adjusted, is stirred to react 15h at 85 DEG C, is cooled to 50 DEG C
Lower natural cooling, suction filtration obtain bulk crystals, obtain the light inhibitor.
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by polytetrahydrofuran ether glycol
14.8g, toluene di-isocyanate(TDI) 53.2g mixing, under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g, in 75 DEG C
Lower reaction 1h, obtains base polyurethane prepolymer for use as A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 DEG C of reaction 2.5h, addition triethylamine 9.4g into
Row neutralization reaction 30min, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g and diethyl is added
Alkene triamine 0.02g, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain light-resistant waterborne polyurethane coating.
Substance B the preparation method comprises the following steps: ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g are stirred at 50 DEG C anti-
1h is answered, 5ml water is added and adjusts pH to 4, the reaction was continued 30min obtains substance B；The equal molecule of the number of the polytetrahydrofuran ether glycol
Amount is 1000；
Embodiment 2
A kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, 2,6- syringol 0.0161g and substance B 0.0012g, are placed in the closed container of 50mL
In, the distilled water of 15g is added, 60min is stirred to react, pH to 5 is adjusted, is stirred to react 21h at 95 DEG C, be cooled at 50 DEG C certainly
So cooling, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by polycarbonate glycol 14.8g, two
Phenylmethane diisocyanate (MDI) 53.2g mixing, under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g, in 80
3h is reacted at DEG C, obtains base polyurethane prepolymer for use as A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 80 DEG C of reaction 2.5h, addition triethylamine 9.4g into
Row neutralization reaction 60min, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g and tetrem is added
Five amine 0.02g of alkene, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain light-resistant waterborne polyurethane coating.
Substance B the preparation method comprises the following steps: ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g are stirred at 60 DEG C anti-
2h is answered, 5ml water is added and adjusts pH to 4, the reaction was continued 30min obtains substance B；The number-average molecular weight of the polycarbonate glycol is
1000。
Embodiment 3
A kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, 3,3- dimethacrylate 0.0161g and substance B 0.0012g, are placed in the closed container of 50mL
In, the distilled water of 15g is added, 45min is stirred to react, pH to 5 is adjusted, is stirred to react 18h at 90 DEG C, be cooled at 50 DEG C certainly
So cooling, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by 1,4-butanediol 14.8g, toluene
Diisocyanate 53.2g mixing reacts 2h at 75 DEG C under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g,
Obtain base polyurethane prepolymer for use as A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 DEG C of reaction 2.5h, addition triethylamine 9.4g into
Row neutralization reaction 45min, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g and diformazan is added
Amido propylamine 0.02g, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain aqueous polyurethane coating.
Substance B the preparation method comprises the following steps: ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g are stirred at 55 DEG C anti-
1.5h is answered, 5ml water is added and adjusts pH to 4, the reaction was continued 30min obtains substance B；
Embodiment 4
A kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, 2,6- syringol 0.0161g and substance B 0.0012g, are placed in the closed container of 50mL
In, the distilled water of 15g is added, 40min is stirred to react, pH to 5 is adjusted, is stirred to react 17h at 90 DEG C, be cooled at 50 DEG C certainly
So cooling, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by polytetrahydrofuran ether glycol
14.8g, '-diphenylmethane diisocyanate 53.2g mixing, under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g, in
2h is reacted at 75 DEG C, obtains base polyurethane prepolymer for use as A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 DEG C of reaction 2.5h, addition triethylamine 9.4g into
Row neutralization reaction 40min, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g and diformazan is added
Amido propylamine 0.02g, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain aqueous polyurethane coating.
Substance B the preparation method comprises the following steps: ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g are stirred at 50 DEG C anti-
1h is answered, 5ml water is added and adjusts pH to 4, the reaction was continued 30min obtains substance B.
Embodiment 5
A kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, chloroacetic acid 0.0161g and substance B 0.0012g, are placed in the closed container of 50mL, then plus
The distilled water for entering 15g is stirred to react 50min, adjusts pH to 5, is stirred to react 20h at 95 DEG C, is cooled to naturally cold at 50 DEG C
But, it filters and obtains bulk crystals, obtain the light inhibitor.
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by polycarbonate glycol 14.8g, first
Phenylene diisocyanate 53.2g mixing is reacted at 75 DEG C under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g
1.5h obtains base polyurethane prepolymer for use as A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 DEG C of reaction 2.5h, addition triethylamine 9.4g into
Row neutralization reaction 40min, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid 0.7g and diethyl is added
Alkene triamine 0.02g, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain light-resistant waterborne polyurethane coating.
Substance B the preparation method comprises the following steps: ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g are stirred at 60 DEG C anti-
1.5h is answered, 5ml water is added and adjusts pH to 4, the reaction was continued 30min obtains substance B；
The number-average molecular weight of the polycarbonate glycol is 2000；
Manufactured polyurethane film is placed in ultraviolet light and aging experimental box (illumination wavelength be 340 nm, 50 DEG C), in sample
Surface is parallel with fluorescent tube bottom surface, distance is the abundant xanthochromia of 24 h of illumination under conditions of 250 mm, after obtaining illumination xanthochromia
Polyurethane film.Using ultraviolet-visible-near infrared spectrometer, the transmitance of polyurethane film is measured.Wavelength scanning range
For 200~800 nm, the present invention selects 450nm measurement (Ren Longfang).
It is detected using spectrophotometer, to obtain inverse difference △ E, to describe the light resistance of coating and finishing coat.△
E represents color change degree, and △ E is bigger, and color change is more obvious.In general, △ E value is the slight change of 0~1.5 category
Change；△ E value is that 1.5~3.0 categories can feel variation；△ E value is 3.0~6.0 category significant changes (referring to Wang Fang, Dang Gaochao, king
Li Qin, light degradation [J] the Northwest University journal of several organic historical relic's protection polymer coatings, 2005,35(5): 56 ~ 58)
1 test data of table
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 24.32 | 26.53 | 25.31 | 15.45 | 13.25 | 32.71 |
| △E/600min | 0.4 | 0.3 | 0.4 | 0.2 | 0.3 | 0.8 |
| Xanthochromia grade | 1.0 | 1.0 | 1.0 | 0.5 | 0.5 | 1.5 |
The embodiment 5 of comparative sample selection 201711369135.5, in terms of above-mentioned data, light resistance of the invention is an advantage over comparative sample
's.
2 test data of table (not plus substance A)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 57.32 | 66.53 | 66.74 | 68.78 | 61.47 | 32.71 |
| △E/600min | 2.1 | 3.2 | 3.3 | 3.9 | 3.1 | 0.8 |
| Xanthochromia grade | 2.5 | 3.0 | 3.0 | 3.0 | 3.0 | 1.5 |
From table 2 it can be seen that not adding the light fastness decline of substance A.
3 test data of table (not plus substance B)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 55.29 | 54.52 | 67.88 | 62.46 | 63.24 | 32.71 |
| △E/600min | 2.2 | 2.1 | 3.5 | 3.3 | 3.7 | 0.8 |
From table 3 it can be seen that not adding the light fastness decline of substance B.
4 test data of table (not plus crosslinking agent)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 31.31 | 31.78 | 37.75 | 34.23 | 33.74 | 32.71 |
From table 4, it can be seen that not adding the performance decline of crosslinking agent.
5 test data of table (add substance B, not plus propionic aldehyde)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 41.32 | 43.55 | 55.12 | 52.36 | 56.41 | 32.71 |
| △E/600min | 1.4 | 1.6 | 2.2 | 2.0 | 2.4 | 0.8 |
As can be seen from Table 5, add substance B and the light resistance of propionic aldehyde is not added to decline.
Claims (8)
1. a kind of preparation method of light-resistant waterborne polyurethane coating, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0471g of the 2,2'- bipyridyl and 0.045g that weigh 0.0356g are anhydrous
Copper sulphate, 0.2416g sodium molybdate, substance A 0.0161g and substance B 0.0012g, are placed in the closed container of 50mL, add
The distilled water of 15g is stirred to react 30 ~ 60min, adjusts pH to 5, is stirred to react 15 ~ 21h at 85 ~ 95 DEG C, is cooled at 50 DEG C certainly
So cooling, suction filtration obtains bulk crystals, obtains the light inhibitor;
(2) equipped with stirring slurry, thermometer, condenser pipe 500ml four-hole boiling flask in, by dihydric alcohol 14.8g, isocyanates
53.2g mixing under the conditions of existing for the catalyst dibutyltin dilaurylate 0.4g, 1 ~ 3h is reacted at 75 ~ 80 DEG C, is gathered
Urethane performed polymer A；
(3) dihydromethyl propionic acid 16.9g is added into base polyurethane prepolymer for use as A, in 75 ~ 80 DEG C of reaction 2.5h, triethylamine is added
9.4g carries out 30 ~ 60min of neutralization reaction, adds water 120g to carry out emulsification 30min, and tetrabutylphosphonium chloride 2.8g, phenyl boric acid is added
0.7g and crosslinking agent 0.02g, 85 DEG C of reaction temperature, reaction time 1h, regulation system pH are 7 ~ 8, obtain aqueous polyurethane coating.
2. a kind of preparation method of light-resistant waterborne polyurethane coating as described in claim 1, substance A is 2- methoxyl group -4-
Any one of methylphenol, 2,6- syringol, 3,3- dimethacrylate, chloroacetic acid.
3. a kind of preparation method of light-resistant waterborne polyurethane coating as described in claim 1, substance B the preparation method comprises the following steps:
Ethylene-ethyl acetate 12g, propionic aldehyde 4.2g, aluminum sulfate 1.4g are stirred to react 1 ~ 2h at 50 ~ 60 DEG C, adds 5ml water and adjusts pH
To 4, the reaction was continued 30min obtains substance B.
4. a kind of preparation method of light-resistant waterborne polyurethane coating as described in claim 1, the dihydric alcohol is poly- four
Any one of hydrogen furans ether glycol, polycarbonate glycol, 1,4- butanediol.
5. a kind of preparation method of light-resistant waterborne polyurethane coating as claimed in claim 4, the polytetrahydrofuran ether two
Any one that the number-average molecular weight of alcohol is 1000,1800,2000.
6. a kind of preparation method of light-resistant waterborne polyurethane coating as claimed in claim 4, the polycarbonate glycol
Any one that number-average molecular weight is 1000 and 2000.
7. a kind of preparation method of the preparation method of light-resistant waterborne polyurethane coating as described in claim 1, the isocyanide
Acid esters is any one of toluene di-isocyanate(TDI) (TDI), '-diphenylmethane diisocyanate (MDI).
8. a kind of preparation method of the preparation method of light-resistant waterborne polyurethane coating as described in claim 1, the crosslinking
Agent is any one of diethylenetriamine, tetraethylenepentamine, dimethylamine propylamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811461308.0A CN109554096A (en) | 2018-12-02 | 2018-12-02 | A kind of preparation method of light-resistant waterborne polyurethane coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811461308.0A CN109554096A (en) | 2018-12-02 | 2018-12-02 | A kind of preparation method of light-resistant waterborne polyurethane coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110591540A (en) * | 2019-09-24 | 2019-12-20 | 安徽国成顺风风力发电有限公司 | Primer for wind driven generator blade |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087149A (en) * | 2014-07-21 | 2014-10-08 | 段宝荣 | Method for preparing light-fast waterborne polyurethane coating material |
| CN105176368A (en) * | 2015-10-26 | 2015-12-23 | 烟台大学 | Preparation method of polyurethane coating and adhesive with flame retardance and light resistance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104087149A (en) * | 2014-07-21 | 2014-10-08 | 段宝荣 | Method for preparing light-fast waterborne polyurethane coating material |
| CN105176368A (en) * | 2015-10-26 | 2015-12-23 | 烟台大学 | Preparation method of polyurethane coating and adhesive with flame retardance and light resistance |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591540A (en) * | 2019-09-24 | 2019-12-20 | 安徽国成顺风风力发电有限公司 | Primer for wind driven generator blade |
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Application publication date: 20190402 |