CN1746236A - High-performance organic-inorganic resin coating material with hybrid acrylic ester and production thereof - Google Patents
High-performance organic-inorganic resin coating material with hybrid acrylic ester and production thereof Download PDFInfo
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Abstract
A high-performance organic-inorganic hybrid acrylate resin coating material and its production are disclosed. The process is carried out by taking inorganic nanometer oxidant collosol containing hydroxyl group and alkoxy as curing agent, reacting with acrylate resin containing functional group, cross-linking and curing to obtain inorganic-organic hybrid coating. It achieves higher hardness, better thermal stability, abrasive and scraping-resistances and ultraviolet shielding characteristic. It can be used for surface protective ornament of car, metal, building, leather and fabric.
Description
Technical field
The present invention relates to chemical industry, field of new, is about a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester and preparation method thereof.
Background technology
Acrylic resin is widely used in the finish paint of automobile, motorcycle, power truck, household electrical appliances, instrument, building, office product and other various metal productss, plastic component, woodwork, paper product etc. owing to the gloss with excellence, the transparency, weathering resistance etc.Traditional acrylic acid coatings material mostly is to form with the acrylic resin that contains functional groups and polyisocyanates or amino resin crosslinked curing, make solidifying agent with polyisocyanates, its residual free HDI, TDI, MDI, IPDI has strong impulse, toxicity, make solidifying agent with aminoresin, then need high bake to solidify, and no matter be to make solidifying agent as solidifying agent or with aminoresin with polyisocyanates, the weathering resistance of coating, temperature tolerance, scale resistance, wear resistance etc. are not very good, all remain further to be improved.
Organic polymer and mineral compound are carried out the above-mentioned performance that organic inorganic hybridization coated material that combining on molecular level or the nano level yardstick form is expected to improve greatly organic polymer coating, and might obtain some new performances at aspects such as calorifics, optics, electricity and electromagnetism, be after single component coated material, composite coating material and gradient cladding material the 4th generation coated material, caused the very big interest of scientific circles and industry member.As patent US5670257 introduced a kind of in acrylic resin the blend polysiloxane prepare the organic inorganic hybridization resin particle, be used for liquid crystal display surface.Patent US6288198 has introduced a kind of isocyanic ester and aminosilane prepared in reaction hybridization coating, is used for surface daub on a walls such as metal, plastics.Patent US5013608 has introduced the preparation method of a kind of siloxanes/SiO 2 hybrid coating, and the hybrid coating material of preparation has high-wearing feature and absorbs ultraviolet function.With nano-oxide colloidal sol is solidifying agent, reacts curing with colloidal sol surface hydroxyl, alkoxyl group and the acrylic resin that contains functional groups, and preparation high-performance organic-inorganic hybrid coating material does not at home and abroad appear in the newspapers as yet.
Summary of the invention
The purpose of this invention is to provide a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester for preparing simple, excellent property and preparation method thereof.
A kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester is to adopt nano-oxide colloidal sol as solidifying agent, with the acrylate resin reaction, and preparation hybrid inorganic-organic coating.The nano-oxide solid content is 1-30wt% in the material, and all the other are acrylate resin, modified resin, color stuffing or auxiliary agent.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, be to adopt nano-oxide colloidal sol and the acrylate resin, modified resin, solvent, color stuffing, the auxiliary agent blend that contain functional group, can obtain organic-inorganic resin coating material with hybrid acrylic ester, film then and carry out self-vulcanizing, or, can obtain the hybrid inorganic-organic coating 20-150 ℃ of scope internal heating curing 0.5-24 hour.Each amounts of components is as follows:
Form weight percent wt%
Nano-oxide colloidal sol 2-60
Acrylate resin 40-98
Modified resin 0-20
Solvent 0-35
Color stuffing 0-15
Auxiliary agent 0-3
Described nano-oxide colloidal sol is that the surface is hydroxyl, the acid inorganic nanometer oxide colloidal sol of alkoxyl group, and acrylate resin is the acrylate resin that contains carboxyl, hydroxyl, epoxy group(ing), alkoxyl group or amide group functional group.
Specifically, organic-inorganic resin coating material with hybrid acrylic ester is made up of nano-oxide colloidal sol, acrylate resin, modified resin, solvent, color stuffing, auxiliary agent, wherein, (1) contains a kind of nano-oxide colloidal sol at least, (2) contain a kind of acrylate resin at least, (3) contain modified resin, (4) contain solvent, color stuffing, auxiliary agent.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, be to adopt acid inorganic nanometer oxide colloidal sol surperficial hydroxyl, alkoxyl group, adopt 1-3 kind wherein, as nano titanic oxide sol, nano-aluminium oxide colloidal sol, nano silicon dioxide sol or nano zircite colloidal sol etc., nano-oxide colloidal sol consumption accounts for the 2-60wt% of total amount.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, be to adopt the acrylate resin that contains carboxyl, hydroxyl, epoxy group(ing), alkoxyl group or amide group functional group, the solid content 30wt%-80wt% of resin, adopt 1-3 kind wherein, with carboxy acrylic ester resin, hydroxyl acrylic resin, epoxy acrylate resin, alkoxy acrylic ester resin, amide group acrylate resin, the acrylate resin consumption accounts for the 40-98wt% of total amount.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, be to adopt modified resin such as silicone resin, urethane resin, vibrin, Resins, epoxy, adopt 1-3 kind wherein, the modified resin consumption accounts for the 0-20wt% of total amount.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, be conventional solvent of employing coating such as varsol, petroleum solvent, alcoholic solvent, esters solvent, ketones solvent, ether solvent, adopt 1-6 kind wherein, as ethanol, butanols, Virahol, acetone, Methyl amyl ketone, methyl ethyl diketone, N-BUTYL ACETATE, ethyl butyrate, solvent oil, dimethylbenzene etc., solvent load accounts for the 0-35wt% of total amount.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, be conventional color stuffing of employing coating such as titanium dioxide, zinc oxide, ferric oxide, aluminum oxide, pearly pigment, aluminium powder, silver powder, pure aluminium silicate, talcum powder, barium sulfate etc., adopt 1-5 kind wherein, the color stuffing consumption accounts for the 0-15wt% of total amount.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes is conventional auxiliary agent of employing coating such as dispersion agent, wetting agent, flow agent, defoamer, anti-settling agent etc., and auxiliary dosage accounts for the 0-3wt% of total amount.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, concrete technology is as follows: in Scattered Kettle, add solvent, auxiliary agent, color stuffing, under the 1000-3000rpm rotating speed, stirred 0.5～1 hour, add acrylate resin again, modified resin, stir, add nano-oxide colloidal sol, under the 300-2000rpm rotating speed, stirred 0.5～3 hour, can obtain organic-inorganic resin coating material with hybrid acrylic ester, film then and carry out self-vulcanizing, or, can obtain the hybrid inorganic-organic coating 20-150 ℃ of scope internal heating curing 0.5-24 hour.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, nano-oxide colloidal sol can be used as the hybrid inorganic-organic coating of novel solidifying agent processability excellence.Useful application is in the surface daub on a wall of automobile, metal, plastics, buildings, stone material, timber, leather or textiles.
The preparation method of a kind of high-performance organic-inorganic resin coating material with hybrid acrylic ester that the present invention proposes, have the following advantages: the present invention adopts the surface hydroxyl, the acid inorganic nanometer oxide colloidal sol of alkoxyl group is novel solidifying agent, with contain carboxyl, hydroxyl, epoxy group(ing), alkoxyl group, the acrylate resin reaction of functional groups such as amide group, crosslinking curing forms the hybrid inorganic-organic coating fast, cross-linking and curing reaction carries out with the volatilization of solvent, need not extra catalyst, in solidification process, by the carboxyl on polymer segment, hydroxyl, epoxy group(ing), alkoxyl group, reactable groups such as amide group and inorganic hydroxyl in mutually, oxyalkylation reaction forms stable covalent linkage, inorganic nanometer oxide is grafted on the acrylate resin segment, both can effectively avoid being separated, the reunion of inorganic nano phase can not appear again, the kind of reactive group and nano-oxide colloidal sol by controlling polymers, consumption, can obtain having the organic-inorganic resin coating material with hybrid acrylic ester of different performance, both ambient temperature curable film forming, also heating curable film forming, it is good both can to have prepared the transparency, the varnish that gloss is high, also can prepare colored paint with good opacifying power and weathering resistance, the hybrid inorganic-organic acrylate resin coating hardness of preparation, thermostability, scoring resistance, wear resistance and uv-shielding capacity etc. all improve a lot, and nano-oxide content can reach more than the 30wt% in the coating.
The high-performance organic-inorganic resin coating material with hybrid acrylic ester of the present invention's preparation, have good decoration effect, hardness, wear resistance, scoring resistance, thermostability and weathering resistance, can be used for the surface daub on a wall of car, metal, plastics, buildings, stone material, timber, leather, textiles etc.
Description of drawings
Fig. 1 is the structural models figure of the acrylate resin hybridized coated material of organic-inorganic nano.R is the functional type group among the figure, and A is a metal or nonmetal.
Embodiment
Embodiment 1:
It is 1 as follows that organic-inorganic resin coating material with hybrid acrylic ester is filled a prescription:
Form weight (gram)
30% nano-titanium oxide colloidal sol 20
30% nano aluminium oxide colloidal sol 10
50% carboxy acrylic ester resin 200
30% alkoxy acrylic ester resin 20
N-BUTYL ACETATE 20
Isophorone 5
1-Methoxy-2-propyl acetate 3
Dimethylbenzene 20
200# solvent oil 2
In Scattered Kettle, add 20 gram N-BUTYL ACETATEs, 5 gram isophorones, 3 gram 1-Methoxy-2-propyl acetates, 20 gram dimethylbenzene, 2 gram 200# solvent oils, the carboxy acrylic ester resin of 200 gram solid contents 50%, the alkoxy acrylic ester resin of 20 gram solid contents 30%, the nano-titanium oxide colloidal sol that under the 500rpm rotating speed, slowly adds 20 grams 30%, 10 grams, 30% nano aluminium oxide colloidal sol, in 30 minutes, add, continue to stir 20 minutes, can prepare hybrid inorganic-organic acrylate coatings material, film, self-vulcanizing 24 hours obtains hybrid inorganic-organic acrylate resin coating.
Nano-oxide content is 3wt% in the coating, gloss (20 ° of Gloss) 94, and pencil hardness 4H, snappiness 1mm, shock strength 50kg/cm manually quickens ageing-resistant time 〉=1000 hour.
Embodiment 2:
It is 2 as follows that organic-inorganic resin coating material with hybrid acrylic ester is filled a prescription:
Form weight (gram)
50% nano oxidized silicon sol 170
80% hydroxyl acrylic resin 120
50% urethane resin 10
Dispersion agent 0.5
Wetting agent 0.6
Flow agent 0.2
In Scattered Kettle, the hydroxyl acrylic resin, 10 grams, 50% urethane resin, 0.5 gram dispersion agent, 0.6 gram wetting agent, the 0.2 gram flow agent that add 120 gram solid contents 80%, the nano oxidized silicon sol that under the 1000rpm rotating speed, slowly adds 170 grams 50%, in 60 minutes, add, continue to stir 30 minutes, can prepare and educate machine-inorganic hybridization acrylate coatings material, film, 70 ℃ solidified 1 hour, and obtained hybrid inorganic-organic acrylate resin coating.
Nano-oxide content is 28wt% in the coating, gloss (20 ° of Gloss) 96, and pencil hardness 5H, snappiness 1mm, shock strength 50kg/cm manually quickens ageing-resistant time 〉=1000 hour.
Embodiment 3:
It is 3 as follows that organic-inorganic resin coating material with hybrid acrylic ester is filled a prescription:
Form weight (gram)
30% nano oxidized silicon sol 50
30% nano zircite colloidal sol 20
30% nano aluminium oxide colloidal sol 10
40% epoxy acrylate resin 20
40% hydroxyl acrylic resin 100
Acetone 45
N-BUTYL ACETATE 25
Virahol 5
Titanium dioxide 12
Aluminium powder 10
Aluminium powder directing agent 2
Dispersion agent 0.1
Defoamer 0.2
Anti-settling agent 0.3
In Scattered Kettle, add 25 gram acetone, 25 gram N-BUTYL ACETATEs, 5 gram Virahols, 12 gram titanium dioxides, 10 gram aluminium powders, 2 gram aluminium powder directing agents, 0.1 gram dispersion agent, 0.2 gram defoamer, 0.3 gram anti-settling agent, high-speed stirring is 30 minutes under the 2000rpm rotating speed, the epoxy acrylate resin that adds 20 gram solid contents 40% again, the hydroxyl acrylic resin of 100 gram solid contents 40%, the nano oxidized silicon sol that under the 1000rpm rotating speed, slowly adds 50 grams 30%, 20 grams, 30% nano zircite colloidal sol, 10 grams, 30% nano aluminium oxide colloidal sol, in 30 minutes, add, continue to stir 20 minutes, can prepare hybrid inorganic-organic acrylate coatings material, film, 90 ℃ solidified 0.5 hour, and obtained hybrid inorganic-organic acrylate resin coating.
Nano-oxide content is 12wt% in the coating, pencil hardness 4H, and snappiness 1mm, shock strength 50kg/cm manually quickens ageing-resistant time 〉=1000 hour.
Embodiment 4:
It is 4 as follows that organic-inorganic resin coating material with hybrid acrylic ester is filled a prescription:
Form weight (gram)
40% nano-titanium oxide colloidal sol 60
40% nano zircite colloidal sol 60
60% amide group acrylate resin 35
70% hydroxyl acrylic resin 100
Vibrin 5
Methyl amyl ketone 20
200# solvent oil 5
Titanium dioxide 7
Barium sulfate 5
Ferric oxide 2
Dispersion agent 0.2
Wetting agent 0.3
Defoamer 0.3
Anti-settling agent 0.2
In Scattered Kettle, add 20 gram Methyl amyl ketones, 5 gram 200# solvent oils, 7 gram titanium dioxides, 5 gram barium sulfate, 2 gram ferric oxide, 0.2 gram dispersion agent, 0.3 gram wetting agent, 0.3 gram defoamer, 0.2 gram anti-settling agent, high-speed stirring is 30 minutes under the 3000rpm rotating speed, add 35 gram solid contents, 60% amide group acrylate resin again, the hydroxyl acrylic resin of 100 gram solid contents 70%, 5 gram vibrin, the nano-titanium oxide colloidal sol that under the 500rpm rotating speed, slowly adds 60 grams 40%, 60 grams, 40% nano zircite colloidal sol, in 30 minutes, add, continue to stir 60 minutes, can prepare hybrid inorganic-organic acrylate coatings material, film, 50 ℃ solidified 12 hours, and obtained hybrid inorganic-organic acrylate resin coating.
Nano-oxide content is 16wt% in the coating, pencil hardness 5H, and snappiness 1mm, shock strength 50kg/cm manually quickens ageing-resistant time 〉=1000 hour.
Embodiment 5:
It is 5 as follows that organic-inorganic resin coating material with hybrid acrylic ester is filled a prescription:
Form weight (gram)
20% nano aluminium oxide colloidal sol 10
50% carboxy acrylic ester resin 50
30% alkoxy acrylic ester resin 80
50% silicone resin 25
50% urethane resin 35
Dimethylbenzene 100
Defoamer 0.1
Flow agent 0.2
In Scattered Kettle, add 100 gram dimethylbenzene, 0.1 gram defoamer, 0.2 gram flow agent, 50 gram solid contents, 50% carboxy acrylic ester resin, the alkoxy acrylic ester resin of 80 gram solid contents 30%, the silicone resin of 25 gram solid contents 50%, the urethane resin of 35 gram solid contents 50%, the nano aluminium oxide colloidal sol that under the 1000rpm rotating speed, slowly adds 10 grams 20%, in 10 minutes, add, continue to stir 20 minutes, can prepare hybrid inorganic-organic acrylate coatings material, film, 80 ℃ solidified 1 hour, and obtained hybrid inorganic-organic acrylate resin coating.
Nano-oxide content is 1.7wt% in the coating, pencil hardness 3H, and gloss (20 ° of Gloss) 95, snappiness 1mm, shock strength 50kg/cm manually quickens ageing-resistant time 〉=1000 hour.
Claims (7)
1. high-performance organic-inorganic resin coating material with hybrid acrylic ester, it is characterized in that adopting nano-oxide colloidal sol to make solidifying agent, with the acrylate resin reaction that contains functional group, preparation hybrid inorganic-organic coating, the nano-oxide solid content is 1-30wt% in the coated material, and all the other are acrylate resin, modified resin, color stuffing or auxiliary agent.
2. the preparation method of a high-performance organic-inorganic resin coating material with hybrid acrylic ester, it is characterized in that nano-oxide colloidal sol and the acrylate resin, modified resin, solvent, color stuffing, the auxiliary agent blend that contain functional group, the preparation organic-inorganic resin coating material with hybrid acrylic ester, further by the self-vulcanizing or the acquisition hybrid inorganic-organic coating that is heating and curing, each amounts of components is as follows:
Form weight percent wt%
Nano-oxide colloidal sol 2-60
Acrylate resin 40-98
Modified resin 0-20
Solvent 0-35
Color stuffing 0-15
Auxiliary agent 0-3
Concrete preparation process is as follows: in Scattered Kettle, add solvent, auxiliary agent, color stuffing, under the 1000-3000rpm rotating speed, stirred 0.5～1 hour, add acrylate resin again, modified resin, stir, add nano-oxide colloidal sol, under the 300-2000rpm rotating speed, stirred 0.5～3 hour, can obtain organic-inorganic resin coating material with hybrid acrylic ester, film then and carry out self-vulcanizing, or 20-150 ℃ of scope internal heating curing 0.5-24 hour, can obtain the hybrid inorganic-organic coating, described nano-oxide colloidal sol is that the surface is hydroxyl, the acid inorganic nanometer oxide colloidal sol of alkoxyl group, acrylate resin is for containing carboxyl, hydroxyl, epoxy group(ing), the acrylate resin of alkoxyl group or amide group functional group.
3. method according to claim 2 is characterized in that the nano-oxide colloidal sol that adopts is nano titanic oxide sol, nano-aluminium oxide colloidal sol, nano silicon dioxide sol, nano zircite colloidal sol, adopts 1-3 kind wherein.
4. method according to claim 2 is characterized in that acrylic resin is carboxyl acrylic resin, Hydroxylated acrylic resin, epoxy acrylic resin, alkoxy propone acid resin or amide group acrylic resin.
5. method according to claim 2 is characterized in that the solid of acrylate resin is divided into 30wt%-80wt%, adopts 1-3 kind wherein.
6. method according to claim 2 is characterized in that modified resin is silicone resin, urethane resin, vibrin or Resins, epoxy, adopts 1-3 kind wherein.
7. the application that high-performance organic-inorganic resin coating material with hybrid acrylic ester according to claim 2 is covered with paint, lacquer, colour wash, etc. as automobile, metal, plastics, buildings, stone material, timber, leather or textile surface.
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