CN110862759A - Foamless fast deep-cured single-component modified PU court material and preparation method thereof - Google Patents
Foamless fast deep-cured single-component modified PU court material and preparation method thereof Download PDFInfo
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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
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
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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
- C08G18/40—High-molecular-weight compounds
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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
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/40—High-molecular-weight compounds
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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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- C09D7/48—Stabilisers against degradation by oxygen, light or heat
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The invention provides a foamless fast deep-cured single-component modified PU court material, which comprises the following components in percentage by weight: polyether polyol: 10 to 30 percent; isocyanate: 2 to 7 percent; filling: 15 to 50 percent; an environment-friendly diluent: 15 to 40 percent; composite stabilizer: 1.5 to 4.5 percent; latent curing agent: 2 to 10 percent; auxiliary agent: 3.42 to 20 percent; the latent curing agent is one or a mixture of more of aldimine, ketimine and oxazolidine. Compared with the silicon PU court in the prior art, the single-component modified PU court material capable of realizing bubble-free rapid deep curing provided by the invention utilizes the latent curing agent to replace an end-capping silane coupling agent, is low in dosage and price, and has the advantages of low TVOC content, convenience and simplicity in construction, high curing speed, bubble-free curing, excellent physical properties and the like.
Description
Technical Field
The invention relates to the field of polyurethane modified materials, in particular to a foamless single-component modified PU court material capable of being rapidly and deeply cured and a preparation method thereof.
Background
The silicon PU has the characteristics of hard middle belt elasticity and elasticity but not softness, and is a professional structure designed for healthy sports. The silicon PU is used for building a court, on one hand, the court rich in hard characteristics can bring professional sports texture, and on the other hand, the court has elastic sports ground, so that the sports buffer can be effectively increased, and the damage of ankles, joints and ligaments of athletes caused by ground reaction force can be reduced; meanwhile, the sport accident injury caused by falling and falling in the sport process is effectively reduced. In addition, the silicon PU also has the characteristics that the silicon PU can be directly constructed on the basis of cement and asphalt, and the surface does not desalt to generate color change. Therefore, the silicon PU is rapidly becoming a healthy professional elastic court material which is uniformly accepted in the market and is popular with the public.
However, the silane coupling agent blocked by silicon PU is expensive, the viscosity of the polymer after blocking can be greatly improved, and the construction can be seriously influenced. The court or runway with the thickness of 8mm can only be constructed for many times by using single-component materials or prepared by using double-component materials according to the current new national standard requirements. However, either method causes a great trouble to the constructor. The single-component material can only be about 2mm in construction thickness at every turn, and bubbles can appear when the construction thickness is too thick at every turn, and the bubbles can lead to the mechanical property greatly reduced of the whole elastic layer. And the single-component material has strict requirements on the environmental temperature, and the construction cannot be carried out when the temperature is too high. The two components are generally an isocyanate component and a hydroxyl component, and need to be accurately blended, so that excessive isocyanate component can cause the effect of more bubbles and swelling, and excessive hydroxyl component can cause the conditions of slow drying, sticky surface and even no drying.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a single-component modified PU court material capable of being rapidly and deeply cured without bubbles and a preparation method thereof, wherein the single-component modified PU court material contains latent curing agent blocked isocyanate, the latent curing agent blocked isocyanate is utilized to rapidly react with water vapor to release amine, the amine then reacts with the isocyanate, the reaction speed of the amine and the isocyanate is much higher than that of water and the isocyanate, the generation of carbon dioxide gas is avoided, the generation of bubbles is avoided, the rapid and deep curing is realized, the technical problem that the mechanical property of the whole elastic layer is greatly reduced due to the generation of bubbles in single-component construction in the prior art is solved, and the problem that the water vapor directly reacts with the isocyanate and is influenced by temperature in the construction process is also avoided.
The technical scheme of the invention is as follows: a single-component modified PU court material capable of being rapidly and deeply cured without bubbles comprises the following components in percentage by weight:
polyether polyol: 10 to 30 percent;
isocyanate: 2 to 7 percent;
filling: 15 to 50 percent;
an environment-friendly diluent: 15 to 40 percent;
composite stabilizer: 1.5 to 4.5 percent;
latent curing agent: 2 to 10 percent;
auxiliary agent: 3.42 to 20 percent;
the latent curing agent is one or a mixture of more of aldimine, ketimine and oxazolidine.
Further, the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 0.5-2%;
coupling agent: 0.5-2%;
water removal agent: 0.2-1%;
catalyst: 0.1 to 1 percent;
flame retardant: 2 to 10 percent;
leveling agent: 0.01-1%;
defoaming agent: 0.01-1%;
dispersing agent: 0.1 to 1 percent;
substrate wetting agent: 0.01-1 percent.
Further, the polyether polyol is one or a mixture of a plurality of polyoxypropylene diol, polyoxyethylene/propylene copolymerized diol, polyoxypropylene triol, polytetrahydrofuran diol, polyolefin polyol and bio-based polyol; wherein the bio-based polyol comprises castor oil and derivatives thereof, soybean oil polyol, palm oil polyol and rosin ester polyol.
Further, the isocyanate is aromatic isocyanate.
Further, the environment-friendly diluent is one or a mixture of a plurality of long-chain chlorinated paraffin, synthetic vegetable ester, citric acid ester and epoxidized soybean oil.
Further, the composite stabilizer is a mixture of an ultraviolet light absorber, a light stabilizer and an antioxidant.
The antioxidant is one or a mixture of more of hindered phenols, aromatic secondary amines and phosphorous acid, wherein the hindered phenols are one of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], triethylene glycol bis- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], isooctyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate or octadecyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate, the aromatic secondary amines are N, N' -bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine or one of butyl and octylated diphenylamine, and the phosphorous acid is tri (2, 4-di-tert-butylphenyl) phosphite;
the ultraviolet light absorber is one or a mixture of a plurality of benzotriazoles, benzophenones and triazines; the benzotriazole is 2- (2 '-hydroxy-3' -tert-butyl-5 '-methylphenyl) -5-chlorobenzotriazole, 2- (2' -hydroxy-3 ', 5' -di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2 '-hydroxy-3', 5 '-di-tert-amylphenyl) benzotriazole, 2- (2' -hydroxy-5 '-methylphenyl) benzotriazole, 2- (2-hydroxy-3-dodecyl-5-methylphenyl) benzotriazole or 2- (2' -hydroxy-3 ', 5' -diphenylisopropyl) benzotriazole; the benzophenone is one of 2-hydroxy-4-octoxybenzophenone; the triazine is 2, 4-bis (2 ', 4' -dimethylphenyl) -6- (2 '-hydroxy-4' -octyloxy) -1,3, 5-triazine;
the light stabilizer is a hindered amine light stabilizer and is selected from one or a mixture of a plurality of poly (1-hydroxyethyl-2, 2,6, 6-tetramethyl-4-hydroxypiperidine) succinate, bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate or a composite light stabilizer Tinuvin PUR68 produced by German BASF.
Further, the coupling agent is one or a mixture of more of epoxy, isocyanate or mercapto silane coupling agents.
Further, the pigment is one or more of phthalocyanine green, iron oxide red, scarlet, phthalocyanine blue, iron green and iron yellow;
the water removing agent is p-toluenesulfonyl isocyanate, triethyl orthoformate and vinyl trimethoxy silane, preferably vinyl trimethoxy silane;
the catalyst is one or a mixture of organic bismuth and organic zinc;
the flame retardant is one or a mixture of a plurality of bromine flame retardants, phosphorus flame retardants and nitrogen non-halogen flame retardants;
the filler is one or a mixture of a plurality of light calcium carbonate, heavy calcium carbonate, modified calcium carbonate, calcined kaolin, talcum powder and silicon micropowder;
the dispersant is a titanate coupling agent, an aluminate coupling agent or a mixture of the two;
the leveling agent is one or a mixture of more of polysiloxane, modified polysiloxane and acrylate copolymer;
the substrate wetting agent is polyether modified polysilane siloxane, polyester modified polysiloxane or a mixture of the polyether modified polysilane siloxane and the polyester modified polysiloxane;
the defoaming agent is one or a mixture of a plurality of polyacrylate, non-organic silicon polymer, polysiloxane and polyether modified organic silicon.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps in sequence:
(1) weighing polyether polyol, isocyanate, a filler, an environment-friendly diluent, a composite stabilizer, a latent curing agent and an auxiliary agent according to the formula amount;
(2) uniformly mixing polyether polyol, an environment-friendly diluent, a filler, a pigment and a dispersing agent, placing the mixture in a reaction kettle, heating to 100-120 ℃, vacuumizing and dehydrating for 0.5-1 h, wherein the vacuum degree is 0.095-0.1 MPa;
(3) cooling the reaction kettle to 50-60 ℃, adding isocyanate and a catalyst, heating to 70-80 ℃ for reaction until the NCO value is 0.5-4%, adding a latent curing agent, continuing to react at 70-80 ℃ for 0.5h, and stopping the reaction when NCO is not detected by titration;
(4) and adding the composite stabilizer, the water removing agent, the coupling agent, the flame retardant, the flatting agent, the base material wetting agent and the defoaming agent into the reaction kettle together, stirring uniformly, and stopping stirring to obtain the single-component modified PU court material.
The invention has the beneficial effects that: compared with the silicon PU court in the prior art, the single-component modified PU court material capable of realizing bubble-free rapid deep curing provided by the invention utilizes the latent curing agent to replace an end-capping silane coupling agent, is low in dosage and price, and has the advantages of low TVOC content, convenience and simplicity in construction, high curing speed, bubble-free curing, excellent physical properties and the like.
The single-component modified PU court material capable of being rapidly and deeply cured without bubbles provided by the invention can be formed at one time to have a thickness of 8mm, can be rapidly and deeply cured without bubbles, and completely meets the requirements of local standards and new national standards.
The single-component modified PU court material provided by the invention belongs to a single component, is convenient and simple to construct, and is less influenced by the environmental temperature in the whole process.
The single-component modified PU court material capable of being rapidly and deeply cured without bubbles provided by the invention is simple in preparation method and easy to implement large-scale production and construction application.
Detailed Description
In order to make the object, technical solution and technical effect of the present invention more apparent, the present invention will be further described with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Embodiment 1 a foamless fast deep-cured single-component modified PU court material, which comprises the following components in percentage by weight:
polyether polyol: 60g of a polyoxyethylene/propylene copolyol (2000 molecular weight), 70g of a polyoxypropylene diol (4000 molecular weight) and 50g of a polyoxypropylene triol (5000 molecular weight);
isocyanate: 31.25g of diphenylmethane diisocyanate;
filling: 401.9g ground calcium carbonate;
an environment-friendly diluent: 235.85g epoxidized soybean oil;
8g of antioxidant tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 8g of ultraviolet light absorber 2- (2-hydroxy-3-dodecyl-5-methyl) benzotriazole, and 8g of light stabilizer bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate);
latent curing agent: 50g Incozol 4 available from Incorez Ltd;
auxiliary agent: 74 g;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of iron oxide red;
coupling agent: 10g of gamma-glycidoxypropyltrimethoxysilane;
water removal agent: 5g of vinyltrimethoxysilane;
catalyst: 2g of organic bismuth;
flame retardant: 40g of dimethyl methylphosphonate;
leveling agent: 3g BYK-S706;
defoaming agent: 3g BYK-A501;
dispersing agent: 5g of diisopropyl di (acetylacetonate) titanate;
substrate wetting agent: 3g BYK-330.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps:
(1) weighing the components according to the formula;
(2) 60g of polyoxyethylene/propylene copolymerized dihydric alcohol (2000 molecular weight), 70g of polyoxypropylene dihydric alcohol (4000 molecular weight), 50g of polyoxypropylene trihydric alcohol (5000 molecular weight), 235.85g of epoxidized soybean oil, 401.9g of heavy calcium carbonate, 6g of iron oxide red and 5g of diisopropyl di (acetylacetone) titanate are added into a dry three-neck flask, dehydrated for 0.5-1 h under the vacuum condition of 120 ℃ and 0.098MPa and cooled to about 60 ℃;
(3) cooling to about 60 ℃, adding 31.25g of metered diphenylmethane diisocyanate and 2g of organic bismuth, slowly heating to 80 ℃ for reaction until the NCO value is tested to be 0.525%, adding 50g of latent curing agent Incozol 4, continuing to react for 0.5h at 72 ℃, and stopping reaction after the NCO is not detected by titration;
(4) adding 8g of antioxidant tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 8g of ultraviolet light absorber 2- (2-hydroxy-3-dodecyl-5-methyl) benzotriazole, 8g of light stabilizer bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate, 5g of water-removing agent vinyl trimethoxy silane, 10g of coupling agent gamma-glycidyl ether oxypropyl trimethoxy silane, 40g of flame retardant dimethyl methyl phosphonate, 3g of flatting agent BYK-S706, 3g of defoaming agent BYK-A50 and 3g of base material wetting agent BYK-330 together, stirring uniformly, stopping stirring, preparing the single-component modified PU court material, and sealing and storing by dry nitrogen.
Example 2:
a foamless fast deep-cured single-component modified PU court material comprises the following components in percentage by weight:
polyether polyol: 80g of a polyoxyethylene glycol (2000 molecular weight), 50g of a polyoxypropylene glycol (4000 molecular weight), 50g of a polyoxypropylene triol (5000 molecular weight);
isocyanate: 33.75g of diphenylmethane diisocyanate;
filling: 411.9g ground calcium carbonate;
an environment-friendly diluent: 218.35g of synthetic vegetable ester;
composite stabilizer: 8g of the antioxidant triethylene glycol bis- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], 8g of the ultraviolet absorber 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-amylphenyl) benzotriazole and 8g of the light stabilizer bis (2,2,6, 6-tetramethyl-4-piperidinyl) sebacate;
latent curing agent: 45g Incozol K available from Incorez Ltd;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of iron green;
coupling agent: 10g of gamma-mercaptopropyltrimethoxysilane;
water removal agent: 5g of vinyltrimethoxysilane;
catalyst: 2g of an organic zinc;
flame retardant: 50g diethyl ethylphosphonate;
leveling agent: 3g BYK-350;
defoaming agent: 3g BYK-A500;
dispersing agent: 5g of titanium di (ethylacetoacetate) diisopropyl ester;
substrate wetting agent: 3g BYK-306.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps:
(1) weighing the components according to the formula;
(2) adding 80g of polyoxyethylene glycol (2000 molecular weight), 50g of polyoxypropylene glycol (4000 molecular weight), 50g of polyoxypropylene triol (5000 molecular weight), 218.35g of synthetic vegetable ester, 411.9g of heavy calcium carbonate, 6g of iron green and 5g of titanium diisopropyl di (ethyl acetoacetate) into a dry three-neck flask, and dehydrating for 0.5-1 h at 120 ℃ under the vacuum of 0.098 MPa;
(3) cooling to about 60 ℃, adding 33.75g of metered diphenylmethane diisocyanate and 2g of organic zinc, slowly heating to 80 ℃ for reaction until the NCO value is tested to be 0.567%, adding 45g of latent curing agent Incozol K, continuing to react for 0.5h at 78 ℃, and stopping titration after NCO is not detected by titration;
(4) adding 8g of antioxidant triethylene glycol bis- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], 8g of ultraviolet light absorber 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-pentylphenyl) benzotriazole, 8g of light stabilizer bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, 5g of water-removing agent vinyl trimethoxy silane, 10g of coupling agent gamma-mercaptopropyl trimethoxy silane, 50g of flame retardant diethyl ethyl phosphonate, 3g of flatting agent BYK-350, 3g of defoaming agent BYK-A500 and 3g of substrate wetting agent BYK-306 together, stirring uniformly, stopping stirring to obtain the single-component modified PU court material, and introducing dry nitrogen for sealed storage.
Example 3:
a foamless fast deep-cured single-component modified PU court material comprises the following components in percentage by weight:
polyether polyol: 70g of polytetrahydrofuran diol (2000 molecular weight), 60g of polyoxypropylene diol (4000 molecular weight), 50g of polyoxypropylene triol (5000 molecular weight);
isocyanate: 32.5g of diphenylmethane diisocyanate;
filling: 360g of ground calcium carbonate;
an environment-friendly diluent: 274.5g of citric acid ester;
composite stabilizer: 8g of antioxidant isooctyl 3, 5-di-tert-butyl-4-hydroxyphenylpropionate, 8g of ultraviolet absorber 2- (2-hydroxy-3-dodecyl-5-methylphenyl) benzotriazole and 8g of light stabilizer Tinuvin PUR 688 g;
latent curing agent: 42g Incozol HP available from Incorez Ltd;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of phthalocyanine blue;
coupling agent: 10g of gamma-isocyanatopropyltrimethoxysilane;
water removal agent: 5g of vinyltrimethoxysilane;
catalyst: 2g of organozinc/organobismuth (1: 1);
flame retardant: 50g triethyl phosphate;
leveling agent: 3g BYK-356;
defoaming agent: 3g BYK-A500;
dispersing agent: 5g of diisopropyl bis (triethanolamine) titanate;
substrate wetting agent: 3g BYK-307.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps:
(1) weighing the components according to the formula;
(2) adding 70g of polytetrahydrofuran dihydric alcohol (2000 molecular weight), 60g of polypropylene oxide dihydric alcohol (4000 molecular weight), 50g of polypropylene oxide trihydric alcohol (5000 molecular weight), 274.5g of citric acid ester, 360g of heavy calcium carbonate, 6g of phthalocyanine blue and 5g of diisopropyl bis (triethanolamine) titanate into a dry three-neck flask, dehydrating for 0.5-1 h at 120 ℃ and under the vacuum of 0.098MPa, and cooling to about 60 ℃;
(3) adding 32.5g of metered diphenylmethane diisocyanate and 2g of organic zinc/organic bismuth (1:1), slowly heating to 80 ℃ for reaction until the NCO value is 0.546 percent, adding 42g of latent curing agent Incozol HP, continuing to react for 0.5h at 70 ℃, and stopping titration after NCO is not detected by titration;
(4) adding 8g of 3, 5-di-tert-butyl-4-hydroxy-iso-octyl phenylpropionate as an antioxidant, 8g of 2- (2-hydroxy-3-dodecyl-5-methylphenyl) benzotriazole as an ultraviolet absorber, 8g of Tinuvin PUR68 as a light stabilizer, 5g of vinyl trimethoxy silane as a water removing agent, 10g of gamma-isocyanate propyl trimethoxy silane as a coupling agent, 50g of triethyl phosphate as a flame retardant, 3g of a flatting agent BYK-356, 3g of a defoaming agent BYK-A550 and 3g of a base material wetting agent BYK-307 together, stirring uniformly, stopping stirring to prepare the single-component modified PU court material, and introducing dry nitrogen for sealed storage.
Example 4:
a foamless fast deep-cured single-component modified PU court material comprises the following components in percentage by weight:
polyether polyol: 50g of a polyolefin diol (1000 molecular weight), 50g of a polyoxypropylene diol (4000 molecular weight), 50g of a polyoxypropylene triol (3000 molecular weight);
isocyanate: 43.75g of diphenylmethane diisocyanate;
filling: 441.9g ground calcium carbonate;
an environment-friendly diluent: 188.35g epoxidized soybean oil;
8g of antioxidant tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 8g of ultraviolet light absorber 2- (2-hydroxy-3-dodecyl-5-methyl) benzotriazole, and 8g of light stabilizer bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate;
latent curing agent: 65g Incozol NC from Incorez Ltd;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of iron oxide red;
coupling agent: 10g of gamma-glycidoxypropyltrimethoxysilane;
water removal agent: 5g of vinyltrimethoxysilane;
catalyst: 2g of organic bismuth;
flame retardant: 50g of dimethyl methylphosphonate;
leveling agent: 3 gBYK-359;
defoaming agent: 3g BYK-A555;
dispersing agent: 5g of isopropyl tris (dodecylbenzenesulfonic acid) titanate;
substrate wetting agent: 3g BYK-333.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps:
(1) weighing the components according to the formula;
(2) adding 50g of polyolefin dihydric alcohol (1000 molecular weight), 50g of polypropylene oxide dihydric alcohol (4000 molecular weight), 50g of polypropylene oxide trihydric alcohol (3000 molecular weight), 188.35g of epoxidized soybean oil, 441.9g of heavy calcium carbonate, 6g of iron oxide red and 5g of isopropyl tri (dodecyl benzene sulfonic acid) titanate into a dry three-neck flask, dehydrating for 0.5-1 h at 120 ℃ and under the vacuum of 0.098MPa, and cooling to about 60 ℃;
(3) adding 43.75g of metered diphenylmethane diisocyanate and 2g of organic bismuth, slowly heating to 80 ℃ for reaction until the NCO value is 0.735%, adding 65g of latent curing agent Incozol NC, continuing to react for 0.5h at 80 ℃, and stopping titration after NCO is not detected by titration;
(4) adding 8g of antioxidant tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester as a composite stabilizer, 8g of ultraviolet light absorber 2- (2-hydroxy-3-dodecyl-5-methyl) benzotriazole, 8g of light stabilizer bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate, 5g of water-removing agent vinyl trimethoxy silane, 10g of coupling agent gamma-glycidyl ether oxypropyl trimethoxy silane, 50g of flame retardant dimethyl methyl phosphonate, 3g of flatting agent BYK-359, 3g of defoaming agent BYK-A555 and 3g of base material wetting agent BYK-333 together, stirring uniformly, stopping stirring to prepare the single-component modified PU court material, and sealing and storing by dry nitrogen.
Example 5:
a foamless fast deep-cured single-component modified PU court material comprises the following components in percentage by weight:
polyether polyol: 30g of castor oil (690 molecular weight), 80g of polyoxypropylene diol (4000 molecular weight), 40g of polyoxypropylene triol (3000 molecular weight);
isocyanate: 49.25g of diphenylmethane diisocyanate;
filling: 400g of ground calcium carbonate;
an environment-friendly diluent: 214.75g of synthetic vegetable ester;
composite stabilizer: 8g of triethylene glycol bis- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] as an antioxidant, 8g of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-amylphenyl) benzotriazole as an ultraviolet absorber, and 8g of bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate as a light stabilizer;
latent curing agent: the weight of 75g of ALT 401,
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of iron green;
coupling agent: 10g of gamma-mercaptopropyltrimethoxysilane;
water removal agent: 5g of vinyltrimethoxysilane;
catalyst: 2g of organic bismuth;
flame retardant: 50g diethyl ethylphosphonate;
leveling agent: 3g BYK-361N;
defoaming agent: 3g BYK-A525;
dispersing agent: 5g of isopropyl trioleate acyloxy titanate;
substrate wetting agent: 3g BYK-341.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps:
(1) weighing the components according to the formula;
(2) 30g of castor oil (690 molecular weight), 80g of polyoxypropylene diol (4000 molecular weight), 40g of polyoxypropylene triol (3000 molecular weight), 214.75g of synthetic vegetable ester, 400g of heavy calcium carbonate, 6g of iron green and 5g of isopropyl trioleate acyloxy titanate are added into a dry three-neck flask, dehydrated for 0.6h at 120 ℃ under the vacuum of 0.098MPa, and cooled to about 60 ℃;
(3) adding 49.25g of metered diphenylmethane diisocyanate and 2g of organic zinc, slowly heating to 80 ℃ for reaction until the NCO value is 0.827%, adding 75g of latent curing agent ALT 401, continuing to react for 0.5h at 70-80 ℃, and stopping titration after NCO is not detected by titration;
(4) adding 8g of composite stabilizer triethylene glycol bis- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], 8g of ultraviolet absorber 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-pentylphenyl) benzotriazole, 8g of light stabilizer bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, 5g of water-removing agent vinyl trimethoxy silane, 10g of coupling agent gamma-mercaptopropyl trimethoxy silane, 50g of flame retardant diethyl ethyl phosphonate, 3g of flatting agent BYK-361N, 3g of defoaming agent BYK-A525 and 3g of base material wetting agent BYK-341 together, stirring uniformly, stopping stirring to obtain the single-component modified PU court material, and introducing dry nitrogen for sealed storage.
Example 6:
a foamless fast deep-cured single-component modified PU court material comprises the following components in percentage by weight:
polyether polyol: 50g of polytetrahydrofuran diol (2000 molecular weight), 80g of polyoxypropylene diol (4000 molecular weight), 40g of polyoxypropylene triol (3000 molecular weight);
isocyanate: 32.5g of diphenylmethane diisocyanate;
filling: 390g ground calcium carbonate;
an environment-friendly diluent: 254.5g of citric acid ester;
composite stabilizer: 8g of antioxidant isooctyl 3, 5-di-tert-butyl-4-hydroxyphenylpropionate, 8g of ultraviolet absorber 2- (2-hydroxy-3-dodecyl-5-methylphenyl) benzotriazole and 8g of light stabilizer Tinuvin PUR 688 g;
latent curing agent: the total weight of 42g of ALT 403,
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of phthalocyanine blue;
coupling agent: 10g of gamma-isocyanatopropyltrimethoxysilane;
water removal agent: 5g of vinyltrimethoxysilane;
catalyst: 2g of organozinc/organobismuth (1: 1);
flame retardant: 50g triethyl phosphate;
leveling agent: 3g BYK-388;
defoaming agent: 3g BYK-A535;
dispersing agent: 5g of isopropyl tris (dioctanoate phosphoryloxy) titanate;
substrate wetting agent: 3g BYK-344.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps:
(1) weighing the components according to the formula;
(2) adding 50g of polytetrahydrofuran dihydric alcohol (2000 molecular weight), 80g of polyoxypropylene dihydric alcohol (4000 molecular weight), 40g of polyoxypropylene trihydric alcohol (3000 molecular weight), 254.5g of citric acid ester, 390g of heavy calcium carbonate, 6g of phthalocyanine blue and 5g of isopropyl tris (dioctanoate phosphoryloxy) titanate into a dry three-neck flask, dehydrating for 0.5-1 h at 120 ℃ and under the vacuum of 0.098MPa, and cooling to about 60 ℃;
(3) adding 32.5g of metered diphenylmethane diisocyanate and 2g of organic zinc/organic bismuth (1:1), slowly heating to 80 ℃ for reaction until the NCO value is 0.546% in the test, adding 42g of latent curing agent ALT 403, continuing to react for 0.5h at 75 ℃, and stopping titration after NCO is not detected by titration;
(4) adding 24g of composite stabilizer (8 g of antioxidant 3, 5-di-tert-butyl-4-hydroxy-iso-octyl phenylpropionate, 8g of ultraviolet light absorber 2- (2-hydroxy-3-dodecyl-5-methylphenyl) benzotriazole, 8g of light stabilizer Tinuvin PUR 688 g), 5g of water-removing agent vinyl trimethoxy silane, 10g of coupling agent gamma-isocyanate propyl trimethoxy silane, 50g of flame retardant triethyl phosphate, 3g of flatting agent BYK-388, 3g of defoaming agent BYK-A535 and 3g of base material wetting agent BYK-344 together, stirring uniformly, stopping stirring to prepare the single-component modified PU court material, and introducing dry nitrogen for sealed storage.
Embodiment 7, a non-foaming fast deep curing single-component modified PU court material, comprising the following components in percentage by weight:
polyether polyol: 100g of soybean oil polyol and 100g of palm oil polyol;
isocyanate: 50g of diphenylmethane diisocyanate;
filling: a mixture of 50g of calcined kaolin and 100g of talc;
an environment-friendly diluent: a mixture of 200g of citrate and 200g of epoxidized soybean oil;
15g of antioxidant tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 15g of ultraviolet light absorber, namely benzotriazole and 15g of light stabilizer bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate;
latent curing agent: 100g of aldimine;
auxiliary agent: 55g of the total weight of the mixture;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 6g of phthalocyanine blue; coupling agent: 6g of isocyanate; water removal agent: 3g of p-toluenesulfonyl isocyanate;
catalyst: 2g of organic zinc; flame retardant: 23g of a nitrogen-based non-halogen flame retardant; leveling agent: 3g of a polysiloxane;
defoaming agent: 2g of a polyacrylate; dispersing agent: 5g of a mixture of a titanate coupling agent and an aluminate coupling agent; substrate wetting agent: 5g of polyether-modified polysilazane.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps in sequence:
(1) weighing polyether polyol, isocyanate, a filler, an environment-friendly diluent, a composite stabilizer, a latent curing agent and an auxiliary agent according to the formula amount;
(2) uniformly mixing polyether polyol, an environment-friendly diluent, a filler, a pigment and a dispersing agent, placing the mixture in a reaction kettle, heating to 110 ℃, vacuumizing and dehydrating for 0.6h, wherein the vacuum degree is 0.095 MPa-0.1 MPa;
(3) cooling the reaction kettle to 55 ℃, adding isocyanate and a catalyst, heating to 75 ℃ for reaction until the NCO value is 3%, adding a latent curing agent, continuing to react at 70 ℃ for 0.5h, and stopping the reaction when NCO is not detected by titration;
(4) and adding the composite stabilizer, the water removing agent, the coupling agent, the flame retardant, the flatting agent, the base material wetting agent and the defoaming agent into the reaction kettle together, stirring uniformly, and stopping stirring to obtain the single-component modified PU court material.
Embodiment 8 a foamless fast deep curing single-component modified PU court material, comprising the following components in percentage by weight:
polyether polyol: 80g of polyoxypropylene triol and 20g of polytetrahydrofuran diol;
isocyanate: 70g of polymethine polyphenyl isocyanate
Filling: a mixture of 200g of light calcium carbonate and 300g of silica micropowder;
an environment-friendly diluent: 100g of long-chain chlorinated paraffin and 100g of synthetic vegetable ester;
composite stabilizer: 5g of thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] as the antioxidant, 5g of 5' -di-tert-amylphenyl) benzotriazole as the ultraviolet light absorber and 5g of Tinuvin PUR68 as a composite light stabilizer produced by BASF in Germany as the light stabilizer; latent curing agent: 80.7g of ketimine; auxiliary agent: 3.43 percent;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 5g of phthalocyanine green; coupling agent: 5g of the coupling agent is a mixture of epoxy acrylic acid and isocyanate; water removal agent: 2g triethyl orthoformate; catalyst: 1g of organic bismuth; flame retardant: 20g of a phosphorus-based non-halogen flame retardant; leveling agent: 0.05g of a polysiloxane and 0.05g of a modified polysiloxane; defoaming agent: 0.1g of polysiloxane; dispersing agent: 1g aluminate coupling agent substrate wetting agent: a mixture of 0.05g of polyether-modified polysiloxane and 0.05g of polyester-modified polysiloxane;
the preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps in sequence:
(1) weighing polyether polyol, isocyanate, a filler, an environment-friendly diluent, a composite stabilizer, a latent curing agent and an auxiliary agent according to the formula amount;
(2) uniformly mixing polyether polyol, an environment-friendly diluent, a filler, a pigment and a dispersing agent, placing the mixture in a reaction kettle, heating to 100 ℃, vacuumizing and dehydrating for 1h, wherein the vacuum degree is 0.095 MPa-0.1 MPa;
(3) cooling the reaction kettle to 50 ℃, adding isocyanate and a catalyst, heating to 70 ℃ for reaction until the NCO value is 0.05%, adding a latent curing agent, continuing to react at 75 ℃ for 0.5h, and stopping the reaction when no NCO is detected by titration;
(4) and adding the composite stabilizer, the water removing agent, the coupling agent, the flame retardant, the flatting agent, the base material wetting agent and the defoaming agent into the reaction kettle together, stirring uniformly, and stopping stirring to obtain the single-component modified PU court material.
Embodiment 9, a non-foaming fast deep curing single-component modified PU court material, comprising the following components in percentage by weight:
polyether polyol: 150g of palm oil polyol and 150g of rosin ester polyol;
isocyanate: 20g of toluene diisocyanate; filling: 100g of modified calcium carbonate 100g of calcined kaolin 70g of talc; an environment-friendly diluent: 150g of the total weight of the mixture; long-chain chlorinated paraffin; composite stabilizer: 10g of the antioxidant tris (2, 4-di-tert-butylphenyl) phosphite; 10g of the ultraviolet light absorber 2-hydroxy-4-octyloxybenzophenone, and 10g of the light stabilizer is hindered amine light stabilizer bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate; latent curing agent: 20g oxazolidine; auxiliary agent: 20 percent;
the auxiliary agent comprises the following components in the total mass of the single-component modified PU court material:
pigment: 20g of bright red; coupling agent: 20g of a mercapto silane coupling agent; water removal agent: 10g of vinyltrimethoxysilane; catalyst: 5g of organobismuth and 5g of organozinc; flame retardant: 100g of a brominated non-halogenated flame retardant; leveling agent: 10g of an acrylate copolymer; defoaming agent: 10g of a mixture of polysiloxane and polyether modified silicone; dispersing agent: 10g titanate coupling agent substrate wetting agent: 10g of polyether-modified polysilazane.
The preparation method of the foamless fast deep-cured single-component modified PU court material comprises the following steps in sequence:
(1) weighing polyether polyol, isocyanate, a filler, an environment-friendly diluent, a composite stabilizer, a latent curing agent and an auxiliary agent according to the formula amount;
(2) uniformly mixing polyether polyol, an environment-friendly diluent, a filler, a pigment and a dispersing agent, putting the mixture into a reaction kettle, heating to 120 ℃, vacuumizing and dehydrating for 0.5h, wherein the vacuum degree is 0.095 MPa-0.1 MPa;
(3) cooling the reaction kettle to 60 ℃, adding isocyanate and a catalyst, heating to 80 ℃ for reaction until the NCO value is 4%, adding a latent curing agent, continuing to react at 80 ℃ for 0.5h, and stopping the reaction when the NCO is not detected by titration;
(4) and adding the composite stabilizer, the water removing agent, the coupling agent, the flame retardant, the flatting agent, the base material wetting agent and the defoaming agent into the reaction kettle together, stirring uniformly, and stopping stirring to obtain the single-component modified PU court material.
And (3) performance testing:
the single-component modified PU court materials prepared in examples 1-6 above, which were foam-free and rapidly cured in the deep layer, were subjected to performance testing, the performance of which is shown in table 1, as follows:
TABLE 1 testing of Properties of the foamless fast deep-curing one-component modified PU court materials prepared in examples 1 to 6
Note: the tensile strength and the elongation at break are tested according to GB/T10654-2001 and total volatile organic compounds GB/T18883-2002.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the present invention pertains, the architecture form can be flexible and varied without departing from the concept of the present invention, and a series of products can be derived. But rather a number of simple derivations or substitutions are made which are to be considered as falling within the scope of the invention as defined by the appended claims.
Claims (10)
1. A single-component modified PU court material capable of being rapidly and deeply cured without bubbles is characterized by comprising the following components in percentage by weight:
polyether polyol: 10 to 30 percent;
isocyanate: 2 to 7 percent;
filling: 15 to 50 percent;
an environment-friendly diluent: 15 to 40 percent;
composite stabilizer: 1.5 to 4.5 percent;
latent curing agent: 2 to 10 percent;
auxiliary agent: 3.42 to 20 percent;
the latent curing agent is one or a mixture of more of aldimine, ketimine and oxazolidine.
2. The one-component modified PU court material capable of being rapidly and deeply cured without bubbles of claim 1, wherein the auxiliary agent comprises the following components in percentage by mass of the total mass of the one-component modified PU court material:
pigment: 0.5-2%;
coupling agent: 0.5-2%;
water removal agent: 0.2-1%;
catalyst: 0.1 to 1 percent;
flame retardant: 2 to 10 percent;
leveling agent: 0.01-1%;
defoaming agent: 0.01-1%;
dispersing agent: 0.1 to 1 percent;
substrate wetting agent: 0.01-1 percent.
3. The foamless fast deep curing one-component modified PU court material of claim 1, wherein the polyether polyol is one or a mixture of several of polyoxypropylene diol, polyoxyethylene/propylene copolymerized diol, polyoxypropylene triol, polytetrahydrofuran diol, polyolefin polyol and bio-based polyol; wherein the bio-based polyol comprises castor oil and derivatives thereof, soybean oil polyol, palm oil polyol and rosin ester polyol.
4. The one-component modified PU court material capable of being rapidly and deeply cured without bubbles of claim 1, wherein the isocyanate is aromatic isocyanate.
5. The one-component modified PU court material capable of being rapidly and deeply cured without bubbles of claim 1, wherein the environmental-friendly diluent is one or a mixture of long-chain chlorinated paraffin, synthetic vegetable ester, citrate and epoxidized soybean oil.
6. The one-component modified PU court material capable of being rapidly and deeply cured without bubbles of claim 1, wherein the composite stabilizer is a mixture of an ultraviolet light absorber, a light stabilizer and an antioxidant.
7. The foamless fast deep-curing one-component modified PU court material of claim 6, wherein the antioxidant is one or more of hindered phenols, secondary aromatic amines and phosphorous acid, wherein the hindered phenols are one or more of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], triethylene glycol bis- [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], isooctyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate or octadecyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate, the secondary aromatic amines are one of N, N' -bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine or butyl, octylated diphenylamine, and the phosphorous acid is tri (2, 4-di-tert-butylphenyl) phosphite;
the ultraviolet light absorber is one or a mixture of a plurality of benzotriazoles, benzophenones and triazines; the benzotriazole is 2- (2 '-hydroxy-3' -tert-butyl-5 '-methylphenyl) -5-chlorobenzotriazole, 2- (2' -hydroxy-3 ', 5' -di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2 '-hydroxy-3', 5 '-di-tert-amylphenyl) benzotriazole, 2- (2' -hydroxy-5 '-methylphenyl) benzotriazole, 2- (2-hydroxy-3-dodecyl-5-methylphenyl) benzotriazole or 2- (2' -hydroxy-3 ', 5' -diphenylisopropyl) benzotriazole; the benzophenone is one of 2-hydroxy-4-octoxybenzophenone; the triazine is 2, 4-bis (2 ', 4' -dimethylphenyl) -6- (2 '-hydroxy-4' -octyloxy) -1,3, 5-triazine;
the light stabilizer is a hindered amine light stabilizer and is selected from one or a mixture of a plurality of poly (1-hydroxyethyl-2, 2,6, 6-tetramethyl-4-hydroxypiperidine) succinate, bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, bis (1,2,2,6, 6-pentamethyl-4-piperidyl) sebacate or a composite light stabilizer Tinuvin PUR68 produced by German BASF.
8. The one-component modified PU court material capable of being rapidly and deeply cured without bubbles of claim 2, wherein the coupling agent is one or a mixture of epoxy, isocyanate or mercapto silane coupling agents.
9. The one-component modified PU court material capable of being rapidly and deeply cured without bubbles of claim 1, wherein the pigment is one or more of phthalocyanine green, iron oxide red, scarlet, phthalocyanine blue, iron oxide green and iron oxide yellow;
the water removing agent is p-toluenesulfonyl isocyanate, triethyl orthoformate and vinyl trimethoxy silane, preferably vinyl trimethoxy silane;
the catalyst is one or a mixture of organic bismuth and organic zinc;
the flame retardant is one or a mixture of a plurality of bromine flame retardants, phosphorus flame retardants and nitrogen non-halogen flame retardants;
the filler is one or a mixture of a plurality of light calcium carbonate, heavy calcium carbonate, modified calcium carbonate, calcined kaolin, talcum powder and silicon micropowder;
the dispersant is a titanate coupling agent, an aluminate coupling agent or a mixture of the two;
the leveling agent is one or a mixture of more of polysiloxane, modified polysiloxane and acrylate copolymer;
the substrate wetting agent is polyether modified polysilane siloxane, polyester modified polysiloxane or a mixture of the polyether modified polysilane siloxane and the polyester modified polysiloxane;
the defoaming agent is one or a mixture of a plurality of polyacrylate, non-organic silicon polymer, polysiloxane and polyether modified organic silicon.
10. The preparation method of the one-component modified PU court material without foam and rapidly solidified in the deep layer according to any one of claims 1 to 9, which comprises the following steps in sequence:
(1) weighing polyether polyol, isocyanate, a filler, an environment-friendly diluent, a composite stabilizer, a latent curing agent and an auxiliary agent according to the formula amount;
(2) uniformly mixing polyether polyol, an environment-friendly diluent, a filler, a pigment and a dispersing agent, placing the mixture in a reaction kettle, heating to 100-120 ℃, vacuumizing and dehydrating for 0.5-1 h, wherein the vacuum degree is 0.095-0.1 MPa;
(3) cooling the reaction kettle to 50-60 ℃, adding isocyanate and a catalyst, heating to 70-80 ℃ for reaction until the NCO value is 1-4%, adding a latent curing agent, continuing to react at 70-80 ℃ for 0.5h, and stopping the reaction when NCO is not detected by titration;
(4) and adding the composite stabilizer, the water removing agent, the coupling agent, the flame retardant, the flatting agent, the base material wetting agent and the defoaming agent into the reaction kettle together, stirring uniformly, and stopping stirring to obtain the single-component modified PU court material.
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| CN113755083A (en) * | 2021-08-01 | 2021-12-07 | 广州励宝新材料科技有限公司 | Preparation method of solvent-free polyurea coating |
| CN113755083B (en) * | 2021-08-01 | 2022-04-15 | 广州励宝新材料科技有限公司 | Preparation method of solvent-free polyurea coating |
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