CN101967350B - Wear-resistant coating material without primer on polycarbonate surface and preparation method thereof - Google Patents
Wear-resistant coating material without primer on polycarbonate surface and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a wear-resistant coating material without a primer on a polycarbonate surface and a preparation method thereof, in particular to a coating material. The invention provides a wear-resistant coating material without a primer on a polycarbonate surface, which can adhere to the polycarbonate surface without the primer, can increase the surface hardness of the polycarbonate plastic and has a wear-resistant function, and a preparation method thereof. The wear-resistant coating material is prepared from at least two functionalities of alkoxy silane and a composition thereof, acidic silica sol, water, an acid catalyst, a diluting agent, polymer polyol, a silane coupling agent, a flatting agent and a curing agent. The preparation method comprises the following steps: mixing the at least two functionalities of alkoxy silane and the composition thereof, the water and the acidic silica sol for reacting; adding the acid catalyst; heating for refluxing; adding the polymer polyol for continuously refluxing; and after cooling, adding the silane coupling agent, the curing agent, the flatting agent and the diluting agent to obtain the wear-resistant coating material without the primer on the polycarbonate surface.
Description
Technical field
The present invention relates to a kind of coated material, especially relate to a kind of polycarbonate surface without abrasion-resistant coating material of primary coat and preparation method thereof.
Background technology
Polycarbonate plastic is compared with opticglass has shock-resistant, the characteristics such as proportion is little, price is low, easy machine-shaping, and developed recently is very fast, but also wear resistance is arranged, the shortcoming such as thermotolerance is relatively poor.Therefore the hardening treatment on polycarbonate and other optical plastics surfaces just seemed particularly important.
The main component of forced fluid is generally silicone resin.Silicone resin polycarbonate surface to adhere to difficulty very large.Usually need to apply first behind the silane coupling agent again the dip-coating silicone resin and just can guarantee silicone resin adhering on the polycarbonate plastic surface.
The Clark of U.S. Dow Corning Corporation is in US Patent No. 3,986,997 have adopted colloid silica and methyltrimethoxy silane hydrolysis, obtained a kind of transparent wear-resistant coating, although the coating that the method obtains is wear-resisting better, but in poor storage stability, the sticking power on polycarbonate is poor, needs silane coupling agent just to have practical value.The said firm discloses a kind of silicone resin that does not need silane coupling agent in Chinese patent 91100464.5, adopted the component of methacrylic hydroxyl ethyl ester class, improved the sticking power of silicone resin on polycarbonate, the coating that obtains is initially adhered on polycarbonate plastic well, but actual hot water resistance can be not good enough.
GE (GE), at US Patent No. P5,503,935, USP5,349, in 002, disclose at room temperature cohydrolysis of employing alkaline silica sol and methyltrimethoxy silane, then added the polyester polyol of hydroxyl or the polymkeric substance of acrylic acid multielement alcohols under the room temperature, to improve the sticking power of silicone resin on polycarbonate, obtained the wear-resistant coating without silane coupling agent.But the silicon sol of alkalescence is adopted in this invention, and behind the silane cohydrolysis, the component that obtains at room temperature stability in storage is bad, becomes easily gel.
Japan day refines (Nippon Fine Chemical Co., Ltd) at US Patent No. P4, has adopted Resins, epoxy as adhesion promoter in 291,098, has obtained being applied to the silicone resin wear-resistant coating without silane coupling agent of polycarbonate surface.But because adopted Resins, epoxy, can not be in the solvent of alcohols dissolve complete, adopt to contain benzene or other solvents, it is unsafe using at airtight dust-free workshop.
William Lewis of the U.S. is at Chinese patent (application number: adopted acid silica sol and Union carbide A-162 96195244.X) under acetic acid catalysis, cohydrolysis when refluxing, added diacetone alcohol as the hangover solvent, apply polycarbonate by secondary, form thin coating at polycarbonate surface, the stress that reduces the contraction generation of coating in the polycarbonate surface drying process obtains higher adhesion property.But such coating in technological operation, needs dip-coating just can reach good adhesion effect twice, and process time consumption is to need not 2 times of the coated material of silane coupling agent, and fraction defective increases about 10%, obviously is uneconomic as industrial application.
Summary of the invention
The purpose of this invention is to provide a kind of silane coupling agent that need not and namely can adhere at polycarbonate surface, the polycarbonate surface that increases the polycarbonate plastic surface hardness and have a wear-resisting functions is without abrasion-resistant coating material of primary coat and preparation method thereof.
Polycarbonate surface of the present invention without raw material composition and the content in mass ratio thereof of the abrasion-resistant coating material of primary coat is:
The organoalkoxysilane of at least two functionality and composition 133～160 thereof;
The acidic silicasol 5～100 of pH=2～6;
Water 0～50;
Acid catalyst 0.002～8;
Thinner 25～100;
Polymer polyatomic alcohol 0.5～10;
Silane coupling agent 5～30;
Flow agent 0.1～1;
Solidifying agent 0.3～2.
The organoalkoxysilane of described at least two functionality and composition thereof can be selected from tetraethoxysilane, tetramethoxy-silicane, Union carbide A-162, methyltrimethoxy silane, phenyl triethoxysilane, methyl triacetoxysilane, dimethylformamide dimethyl oxygen alkane, dimethyl diethoxy alkane, at least a in the silicone oil etc.
Described acidic silicasol can be the acidic silicasol of pH=2～6, and particle diameter is preferably 10～20nm at 5～50nm.
Described acidic silicasol can adopt the organic solvent type silicon sol of acid water silica sol or acidity etc., the water silica sol of preferred acidic.
Described acid catalyst is preferred 0.005～8, and described acid catalyst can be selected from nitric acid, sulfuric acid, hydrochloric acid, acetic acid, p-methyl benzenesulfonic acid, a kind of in the acetic acid etc.
Described thinner can be the organic solvent of boiling point between 60～150 ℃, and the solvent that its mid-boiling point is higher than more than 90 ℃ preferably is no less than 5; Described organic solvent can adopt ethanol, Virahol, butanols, ethylene glycol ethyl ether, butyl glycol ether, propylene glycol monomethyl ether, isopropylcarbinol, diacetone alcohol, tetrahydrofuran (THF), at least a in the DMF etc.
Described polymer polyatomic alcohol can be the polymkeric substance that comprises 2 or 3 hydroxyls, number-average molecular weight between 300～10000, a kind of in the optional self-polycarbonate polyvalent alcohol of described polymer polyatomic alcohol, poly adipate succinic acid ester polyvalent alcohol, poly-propylene oxide polyvalent alcohol, the polytetrahydrofuran polyvalent alcohol etc.
Described silane coupling agent can adopt at least a in γ aminopropyltriethoxy silane, gamma-amino propyl group methyl dimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane etc.
Described flow agent can adopt a kind of in polydimethylsiloxane, polyester-modified polysiloxanes, the Siloxane-Oxyalkylene Copolymers etc.
Described solidifying agent can be selected from tertiary amine, quaternary ammonium, at least a in the metal alkoxide etc., described tertiary amine can adopt N, N-dimethyl benzylamine or triethylamine etc., described quaternary ammonium can adopt Tetramethylammonium hydroxide, TBAH, the tetramethyl-ammonium acetate, a kind of in the tetramethyl ammonium chloride etc., described metal alkoxide can be selected from aluminum isopropylate, titanium isopropylate, aluminium acetylacetonate, a kind of in the aluminium secondary butylate etc.
Polycarbonate surface of the present invention may further comprise the steps without the preparation method of the abrasion-resistant coating material of primary coat:
1) organoalkoxysilane and composition, water and the acidic silicasol with at least two functionality joins hybrid reaction in the reactor;
2) after system becomes transparent and homogeneous, add acid catalyst, temperature rising reflux adds polymer polyatomic alcohol and continues to reflux, and then is cooled to room temperature;
3) add silane coupling agent, solidifying agent, flow agent and thinner, obtain polycarbonate surface without the abrasion-resistant coating material of primary coat, product is the outward appearance micro emulsion and is clear in vain translucent liquid, can be directly used in the dip-coating without the polycarbonate of primary coat.
In step 1) in, the mass ratio of the organoalkoxysilane of described at least two functionality and composition thereof, water and acidic silicasol can be organoalkoxysilane and the composition thereof of at least two functionality: water: acidic silicasol=(133～160): (0～50): (5～100); The temperature control of described reaction is below 60 ℃; Described acidic silicasol can adopt the acidic silicasol of pH=2～6, and particle diameter can be 5～50nm, is preferably 10～20nm; Described water can adopt deionized water.
In step 2) in, the amount of described adding acid catalyst and the mass ratio of acidic silicasol can be (0.005～2): (5～70): (0.002～8): (5～100); The time of described temperature rising reflux can be 0.5～4h; The time that described adding polymer polyatomic alcohol continues later on to reflux can be 0.5～2h; Described acid catalyst can adopt a kind of in nitric acid, sulfuric acid, hydrochloric acid, acetic acid, the p-methyl benzenesulfonic acid etc.; Described polymer polyatomic alcohol can adopt the polymkeric substance that comprises 2 or 3 hydroxyls, number-average molecular weight between 300～10000, a kind of in preferred polymer polyatomic alcohol such as polycarbonate polyol, poly adipate succinic acid ester polyvalent alcohol, poly-propylene oxide polyvalent alcohol, the polytetrahydrofuran polyvalent alcohol etc.
In step 3) in, the add-on of described silane coupling agent, solidifying agent, flow agent and thinner and the mass ratio of acidic silicasol can be silane coupling agent: solidifying agent: flow agent: thinner: acidic silicasol=(5～30): (0.3～2): (0.1～1): (25～100): (5～100); Described thinner can adopt the organic solvent of boiling point between 60～150 ℃, and described organic solvent can adopt ethanol, Virahol, butanols, ethylene glycol ethyl ether, butyl glycol ether, propylene glycol monomethyl ether, isopropylcarbinol, diacetone alcohol, tetrahydrofuran (THF), N, at least a in the dinethylformamide etc., the organic solvent that described thinner mid-boiling point is higher than more than 90 ℃ preferably can not be less than 5 parts; Described solidifying agent can be selected from tertiary amine, quaternary ammonium, at least a in the metal alkoxide etc., described tertiary amine can adopt N, N-dimethyl benzylamine or triethylamine etc., described quaternary ammonium can adopt Tetramethylammonium hydroxide, TBAH, the tetramethyl-ammonium acetate, a kind of in the tetramethyl ammonium chloride etc., described metal alkoxide can be selected from aluminum isopropylate, titanium isopropylate, aluminium acetylacetonate, a kind of in the aluminium secondary butylate etc.
Organosilicon stiffened abrasion-resistant coating material outward appearance micro emulsion provided by the invention is white translucent to the translucent liquid shape, does not need during dip-coating in advance polycarbonate surface to be carried out pre-treatment, and implementing process is simple, and is efficient.
After tested, can satisfy existing resin lens client's following requirement:
1) but do not need the silane coupling agent dip-coating;
2) 50～70 ℃ of prebake 10～20min, 120 ℃ of lower 120min solidify;
3) coating that obtains is initially adhered to hundred lattice and is not come off;
4) coating is after 80 ℃ of hot water boil 30min, and the surface is without unusual, and hundred lattice do not come off;
5) 0000# Steel Wool, 500g counterweight load is lower, scratches through 20 back and forth friction nothings;
6) coated material at least room temperature preservation after 90 days performance substantially remain unchanged.
Embodiment
The below enumerates embodiment the present invention is specifically described, and only the present invention is further illustrated to it is important to point out embodiment, can not be interpreted as limiting the scope of the invention.
Embodiment 1
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 36g, Union carbide A-162 133g, tetraethoxysilane 6g, dimethyldiethoxysilane 6g, deionized water 15g becomes transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then adds acetic acid 3g, be warmed up to 82 ℃ of back flow reaction 2h, under 82 ℃, adding molecular weight is 1000 PCDL 6g, continues reaction 30min, cooling, then in the time of 50 ℃, add γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane 12g, behind the cool to room temperature, add at last Virahol 70g, butyl glycol ether 18g, organosilicon flow agent 0.5g, tetrabutylammonium acetate ammonium 0.5g, obtain the organic silicon wear resistance coating material, be designated as A1.
With thick 1mm, long 110mm, the polycarbonate plate of wide 40mm, immerse in the above-mentioned coated material, at the uniform velocity lift vertically upward with the speed of 25cm/min, put into 60 ℃ hot-air oven, behind the 10min, temperature is elevated to 120 ℃, behind 120min, obtains the wear-resistant coating that uniform thickness is about 2-5 μ m.
The polycarbonate plate that wear-resistant coating protection is arranged, be placed under the 0000# Steel Wool of 500g counterweight load, 20 of mobile polycarbonate plates are observed the surface tear situation back and forth.The 0-5 bar scratches, and is designated as excellently, and the 5-20 bar scratches, be designated as good, scratch more than 20 be designated as poor.
Having on the polycarbonate plate of wear-resistant coating, in the scope of 25.4mm * 25.4mm, 10 grooves of each stroke are drawn 100 lattices altogether in length and breadth, glue 3 times observation coating shedding situation with the 3M610 adhesive tape.100% does not come off, and is designated as OK, and 1% above area comes off, and is designated as NG.
To test the coating of initially adhering to, put into 80 ℃ warm water, boil 30min after, the cooling, repeat the above-mentioned test of adhering to.100% does not come off, and is designated as OK, and 1% above area comes off, and is designated as NG.
Embodiment 2
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 70g, Union carbide A-162 133g, become transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then add acetic acid 3g, be warmed up to 82 ℃ of back flow reaction 2h, under 82 ℃, the adding molecular weight is 800 PCDL 2.7g, continue reaction 30min, then cooling adds γ-(2 in the time of 50 ℃, 3-epoxy the third oxygen) propyl trimethoxy silicane 20g, behind the cool to room temperature, add at last Virahol 90g, butyl glycol ether 25g, organosilicon flow agent 0.2g, TBAH 0.5g has obtained the organic silicon wear resistance coating material, is designated as A2.
Embodiment 3
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 6g, Union carbide A-162 133g, deionized water 36g becomes transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then add 1% aqueous hydrochloric acid 0.5g, be warmed up to 82 ℃ of back flow reaction 2h, under 82 ℃, the adding molecular weight is 2000 polytetrahydrofuran dibasic alcohol 2.7g, continue reaction 30min, then cooling adds γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane 12g in the time of 50 ℃, behind the cool to room temperature, add at last Virahol 90g, butyl glycol ether 20g, organosilicon flow agent 0.2g, N, N-dimethyl benzylamine 0.5g has obtained the organic silicon wear resistance coating material, is designated as A3.
Embodiment 4
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 70g, Union carbide A-162 133g, become transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then add acetic acid 3g, be warmed up to behind 82 ℃ of back flow reaction 4h under 82 ℃, the adding molecular weight is 800 PCDL 3.0g, continues to cool off behind the reaction 30min, then adds γ-(2 in the time of 50 ℃, 3-epoxy the third oxygen) propyl trimethoxy silicane 12g, behind the cool to room temperature, add at last Virahol 90g, butyl glycol ether 20g, TBAH 0.5g, organosilicon flow agent 0.2g has obtained the organic silicon wear resistance coating material, is designated as A4.
Embodiment 5
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 100g, Union carbide A-162 133g, become transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then add acetic acid 3g, be warmed up to 82 ℃ of back flow reaction 0.5h, under 82 ℃, adding molecular weight is PCDL 9g, continue reaction 30min, then cooling adds γ-(2 in the time of 50 ℃, 3-epoxy the third oxygen) propyl trimethoxy silicane 25g, behind the cool to room temperature, add at last Virahol 80g, butyl glycol ether 20g, TBAH 0.5g, organosilicon flow agent 0.2g has obtained the organic silicon wear resistance coating material, is designated as A5.
Comparative Examples 1
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 6g, Union carbide A-162 133g, deionized water 36g, acetic acid 4g, at room temperature stirred 7 days, and then added γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane 12g, behind the cool to room temperature, add at last Virahol 90g, butyl glycol ether 20g, N, N-dimethyl benzylamine 0.5g has obtained the organic silicon wear resistance coating material, is designated as B1.
Comparative Examples 2
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 5g, Union carbide A-162 133g, water 35g, become transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then add acetic acid 3g, be warmed up to that to add molecular weight behind 82 ℃ of back flow reaction 2h be 1000 PCDL 6g, continue reaction 30min, cooling adds Virahol 80g, butyl glycol ether 20g after room temperature, TBAH 0.5g, organosilicon flow agent 0.2g has obtained the organic silicon wear resistance coating material, is designated as B2.
Comparative Examples 3
In three mouthfuls of round-bottomed flasks of a 250ml, add pH=2, solid content is 34% acidic silicasol 6g, Union carbide A-162 133g, water 35g, dimethyldiethoxysilane 20g, become transparent and homogeneous to get component after about hydrolysis nature thermopositive reaction to 40 ℃, then add acetic acid 3g, cool off after being warmed up to 82 ℃ of back flow reaction 2h, then in the time of 50 ℃, add γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane 12g, behind the cool to room temperature, add at last Virahol 80g, butyl glycol ether 10g, TBAH 0.5g, organosilicon flow agent 0.2g has obtained the organic silicon wear resistance coating material, is designated as B3.
Different embodiment wear-resisting and adhering to, and the water boiling resistance performance is referring to table 1.
Table 1
| The prescription number | Wear-resisting | Initially adhere to | Test behind 80 ℃ of poach 30min and adhere to |
| A1 | Excellent | Excellent | Excellent |
| A2 | Excellent | Excellent | Excellent |
| A3 | Very | Excellent | Excellent |
| A4 | Excellent | Excellent | Excellent |
| A5 | Excellent | Excellent | Excellent |
| B1 | Very | NG | NG |
| B2 | Very | NG | NG |
| B3 | Very | Excellent | NG |
Claims (9)
1. polycarbonate surface is characterized in that without the abrasion-resistant coating material of primary coat its raw material forms and content in mass ratio is:
The organoalkoxysilane of at least two functionality and composition 133～160 thereof;
The acidic silicasol 5～100 of pH=2～6;
Deionized water 0～50;
Acid catalyst 0.002～8;
Thinner 25～100;
Polymer polyatomic alcohol 0.5～10;
Silane coupling agent 5～30;
Flow agent 0.1～1;
Solidifying agent 0.3～2;
Organoalkoxysilane and the composition thereof of described at least two functionality are selected from tetraethoxysilane, tetramethoxy-silicane, Union carbide A-162, methyltrimethoxy silane, phenyl triethoxysilane, methyl triacetoxysilane, dimethylformamide dimethyl oxygen alkane, dimethyl diethoxy alkane, at least a in the silicone oil;
Described silane coupling agent is at least a in γ-aminopropyltriethoxywerene werene, γ-aminopropyl methyl dimethoxysilane, γ-mercaptopropyltriethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane.
2. polycarbonate surface as claimed in claim 1 is characterized in that without the abrasion-resistant coating material of primary coat described acidic silicasol is the acidic silicasol of pH=2～6, and particle diameter is at 5～50nm; Described acidic silicasol adopts acid water silica sol or acid organic solvent type silicon sol.
3. polycarbonate surface as claimed in claim 2 is characterized in that without the abrasion-resistant coating material of primary coat described particle diameter is 10～20nm; Described acidic silicasol adopts acid water silica sol.
4. polycarbonate surface as claimed in claim 1 is characterized in that without the abrasion-resistant coating material of primary coat described acid catalyst is 0.005～8, and described acid catalyst is selected from nitric acid, sulfuric acid, hydrochloric acid, acetic acid, a kind of in the p-methyl benzenesulfonic acid;
Described thinner is the organic solvent of boiling point between 60～150 ℃, and the solvent that its mid-boiling point is higher than more than 90 ℃ is no less than 5; Described organic solvent is selected from ethanol, Virahol, butanols, ethylene glycol ethyl ether, butyl glycol ether, propylene glycol monomethyl ether, isopropylcarbinol, diacetone alcohol, tetrahydrofuran (THF), at least a in the DMF.
5. polycarbonate surface as claimed in claim 1 is without the abrasion-resistant coating material of primary coat, it is characterized in that described polymer polyatomic alcohol is the polymkeric substance that comprises 2 or 3 hydroxyls, number-average molecular weight is between 300～10000, and described polymer polyatomic alcohol is selected from a kind of in polycarbonate polyol, poly adipate succinic acid ester polyvalent alcohol, poly-propylene oxide polyvalent alcohol, the polytetrahydrofuran polyvalent alcohol.
6. polycarbonate surface as claimed in claim 1 is without the abrasion-resistant coating material of primary coat, it is characterized in that described flow agent is selected from a kind of in polydimethylsiloxane, polyester-modified polysiloxanes, the Siloxane-Oxyalkylene Copolymers.
7. polycarbonate surface as claimed in claim 1 is characterized in that without the abrasion-resistant coating material of primary coat described solidifying agent is selected from tertiary amine, quaternary ammonium, at least a in the metal alkoxide, described tertiary amine is N, N-dimethyl benzylamine or triethylamine, described quaternary ammonium is Tetramethylammonium hydroxide, TBAH, tetramethyl-ammonium acetate, a kind of in the tetramethyl ammonium chloride, described metal alkoxide is selected from aluminum isopropylate, titanium isopropylate, aluminium acetylacetonate, a kind of in the aluminium secondary butylate.
8. polycarbonate surface as claimed in claim 1 is characterized in that may further comprise the steps without the preparation method of the abrasion-resistant coating material of primary coat:
1) organoalkoxysilane and composition, water and the acidic silicasol with at least two functionality joins hybrid reaction in the reactor;
2) after system becomes transparent and homogeneous, add acid catalyst, temperature rising reflux adds polymer polyatomic alcohol and continues to reflux, and then is cooled to room temperature;
3) add silane coupling agent, solidifying agent, flow agent and thinner, obtain polycarbonate surface without the abrasion-resistant coating material of primary coat, product is the outward appearance micro emulsion and is clear in vain translucent liquid, can be directly used in the dip-coating without the polycarbonate of primary coat.
9. polycarbonate surface as claimed in claim 8 is characterized in that in step 1) without the preparation method of the abrasion-resistant coating material of primary coat, and the temperature of described reaction is to be controlled at below 60 ℃; In step 2) in, the time of described temperature rising reflux is 0.5～4h; The time that described adding polymer polyatomic alcohol continues later on to reflux is 0.5～2h.
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| CN101967350A (en) | 2011-02-09 |
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