CN106833169A - The preparation method and application of the long-acting antifog clear coat of high intensity - Google Patents
The preparation method and application of the long-acting antifog clear coat of high intensity Download PDFInfo
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- CN106833169A CN106833169A CN201710021406.1A CN201710021406A CN106833169A CN 106833169 A CN106833169 A CN 106833169A CN 201710021406 A CN201710021406 A CN 201710021406A CN 106833169 A CN106833169 A CN 106833169A
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- C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/02—Homopolymers or copolymers of unsaturated alcohols
- C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
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- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a kind of preparation method of the long-acting antifog clear coat of high intensity, the method includes：The polymer powder that main chain or side chain contain hydrophilic radical is mixed with water, solution is prepared；Resulting solution is stirred under the bath temperature that temperature is 10~70 DEG C, organosilane reagents are added, inorganic acid is added, regulation pH value of solution continues to stir to 1~7, and organo silane coupling agent is added after solution is transparent, stirring, stands at room temperature, obtains long-acting antifog sol solutionses；Resin lens are placed in long-acting antifog sol solutionses, are impregnated, then slowly taken out, placed, dried in an oven, then cool down 2~10min at a temperature of 20~15 DEG C rapidly, obtain the long-acting antifog clear coat of high intensity；Wherein, the temperature of drying is 160~200 DEG C, and the time of drying is 2~240min.The method is simple, and the coating for obtaining has excellent long-acting anti-fog performance and mechanical strength, is combined the standard that actual industrial metaplasia is produced.
Description
Technical field
The present invention relates to Material Field.More particularly, to a kind of preparation method and application of long-acting antifog clear coat.
Background technology
Amino containing hydrophilic functional group, urea groups, sulfydryl, hydroxyl, azanol base, carboxyl, the polymer such as amino of ester group gather
Compound, polyureas, sulfydryl polymer, polyvinyl alcohol, polymeric hydroxylamine, polyethylene glycol, polycarboxylic acids, polyvinyl acetate, antifog
Frost-resistant field has a wide range of applications.But these polymer are dissolved in water, it is impossible to individually used as antifog frost-resistant coating.Will
Reach long-acting anti-fog properties and excellent coating stability and water resistance, in addition it is also necessary to which the structure to polymer carries out certain changing
Journal of Sex Research.Wherein, constructing polymer network structure is a kind of preferable method (Pascal C.Applied Materials＆
Interfaces.2011,3,750-758).In existing research, have to be modified PVA by using formaldehyde is carried out to it again
The pollution that the use so as to obtain formaldehyde in nonpolluting coating, but the method easily causes environment, and influence health are crosslinked, are prepared
Process needs multistep, is not suitable for large-scale industrial production；Contain the poly- of hydroxyl also by crosslinking, control main chain or side chain
The hydroxyl bonding rate of compound obtains water-fast antifog frost-resistant coating, but the coating that obtains of these specific schemes is water-fast antifog
Although frost-resistant performance can be improved, the actual strength of coating for obtaining is extremely difficult to the demand of enterprise practical application
Standard.
Optical resin lens are a kind of organic materials, and it is the mirror after being polished as raw material chemical process synthesis with resin
Piece, has important effect in real life, but the heat distortion temperature of resin lens is relatively low, so as to the coating to its surface
Also there is requirement higher.How to enable that coating is firmly combined with resin lens, and ensure what the coating can also have
Anti-fog performance and strong mechanical performance also need to further research.
Accordingly, it is desirable to provide a kind of preparation method of new coating, to solve the above problems.
The content of the invention
First purpose of the invention is to provide a kind of preparation method of long-acting antifog clear coat.
Second object of the present invention is to provide a kind of coating that above-mentioned preparation method prepares in resin lens
Application.
To reach above-mentioned first purpose, the present invention uses following technical proposals：
The preparation method of the long-acting antifog clear coat of high intensity, the preparation method comprises the following steps：
1) polymer powder that main chain or side chain are contained into hydrophilic radical mixes with water, be configured to mass concentration for 5%~
25% aqueous solutions of polymers；
2) by step 1) aqueous solutions of polymers that obtains stirs 30 under the bath temperature that temperature is 10~70 DEG C~
720min, adds organosilane reagents, adds inorganic acid, and regulation pH value of solution to 1~7 continues to stir 30~720min, treats molten
Organo silane coupling agent is added after liquid is transparent, stirring stands at room temperature, obtains long-acting antifog sol solutionses；
3) resin lens are placed in step 2) in the long-acting antifog sol solutionses that obtain, impregnate 5~120s, then slowly take
Go out, place 2~10min, dry in an oven, then cool down 2~10min at a temperature of -20~15 DEG C rapidly, obtain high intensity long
Imitate antifog clear coat；Wherein, the temperature of drying is 160~200 DEG C, and the time of drying is 2~240min.
In the present invention, step 2) in organosilane reagents or the addition of organo silane coupling agent can be 0, but both are not
Can be simultaneously 0；Preferably, step 2) in, the addition of organosilane reagents and organo silane coupling agent is according to step 1) in institute
The amount of the material of hydrophilic radical and the material of organosilane reagents in the polymer that the main chain or side chain stated contain hydrophilic radical
The ratio of amount is 5:1~1:0, in the polymer that described main chain or side chain contains hydrophilic radical the amount of the material of hydrophilic radical with have
The ratio of the amount of the material of machine silane coupling agent is 20:1~1:20.
Preferably, step 2) in, the addition of organosilane reagents and organo silane coupling agent is according to step 1) described in
Main chain or side chain contain hydrophilic radical polymer in hydrophilic radical material amount and described organosilane reagents and have
The ratio of the amount of total material of machine silane coupling agent is 5:1~20:1.
The mixture homogeneity of the sol solutionses that the control influence of bath temperature is obtained in the application, when bath temperature control is 10
At~70 DEG C, can cause that sol solutionses mix more uniform.Preferably, when bath temperature is 55~70 DEG C, foregoing advantages are more preferably.
Inventor is found surprisingly that in research process, will impregnate the resin lens after long-acting antifog sol solutionses in an oven
Drying temperature when being increased to 160~200 DEG C, can greatly improve coating intensity and its combined with resin lens it is firm
Degree.Preferably, drying temperature is 170~190 DEG C, and when drying time is 5~60min, the improvement result to foregoing advantages is brighter
It is aobvious.Further, drying temperature can also be such as 182~190 DEG C, 170~180 DEG C etc..
Controlling drying temperature under conditions of 160~200 DEG C, inventor is it has furthermore been found that by the resin mirror after drying
The rapid cooling in a low temperature of -20~15 DEG C of piece can further improve the anti-fog properties and antifog long-lasting, saturating of gained coating
Bright property and mechanical strength.Preferably, chilling temperature is -20~0 DEG C, and cool time is 2~5min, and now foregoing advantages are changed
Kind effect is more preferably.Further, chilling temperature can also be -20~-5 DEG C, -20~-8 DEG C, -18~-5 DEG C, -15~-10 DEG C etc..
Preferably, the main chain or side chain contain hydrophilic radical in the polymer of hydrophilic radical be amino, urea groups, sulfydryl,
Hydroxyl, azanol base, carboxyl or ester group.
Preferably, the polymer that the main chain or side chain contain hydrophilic radical is selected from amino polymer, polyureas, sulfydryl polymerization
In thing, polyvinyl alcohol, polymeric hydroxylamine, polyethylene glycol, polycarboxylic acids, polyvinyl acetate, polyethyleneglycol block copolymer one
Plant or several.
Preferably, the organosilane reagents are selected from APTES, 3- mercaptopropyi triethoxies
In silane, MTMS, tetramethoxy-silicane, tetraethyl orthosilicate, positive silicic acid propyl ester and positive isopropyl silicate one
Plant or several.
Preferably, the organo silane coupling agent is selected from γ-aminopropyltrimethoxysilane, aminopropyl-triethoxy silicon
Alkane, 3- glycydoxies trimethoxy silane, γ-methacryloxypropyl trimethoxy silane, vinyl
Triethoxysilane, vinyltrimethoxy silane, ('beta '-methoxy ethyoxyl) silane of vinyl three and N- (β-aminoethyl)-
One or more in gamma-aminopropyl-triethoxy-silane.
Preferably, the inorganic acid is selected from one or more in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
Preferably, step 2) in, the time of the standing is 0.5~36h.
Preferably, step 3) in, the resin lens are first pre-processed before dipping to resin lens, pretreatment
Method is：With oxygen plasma in 600~800V, 5~10min is cleaned under 800~1200mL/min throughputs.To resin lens
After carrying out oxygen plasma pretreatment, may be such that resin lens can be combined preferably with sol solutionses.
To reach above-mentioned second purpose, it is long-acting antifog that the present invention also provides the high intensity that above-mentioned preparation method prepares
Application of the clear coat in resin lens.
The above-mentioned coating for preparing is used as the coating of resin lens, the anti-fog properties, anti-of resin lens can be improved
Long-lasting and transparency of mist etc..
Each raw material used can be obtained by the commercially available purchase of business unless otherwise specified in the present invention.Except described above
Outward, the operation and device therefor being not specifically mentioned in preparation method of the invention can be using the conventional equipments in art
Or with reference to being carried out in the prior art in the field, and methods described is unless otherwise specified, is conventional method.
Beneficial effects of the present invention are as follows：
The coating that preparation method of the invention is obtained has extremely high performance mechanical strength, and with excellent long-acting
Anti-fog performance, meets the standard of actual industrial metaplasia product.Wherein, mechanical strength：Determined using pencil hardness method, hardness reaches
8H；Anti-fog performance：Anti-fog performance：Temperature be 70 DEG C, humidity be 95% in the environment of do not haze within 2 hours；At a temperature of -30 DEG C
Frost 30 hours, does not haze at room temperature.Firmness performance：Hundred lattice are marked in coating surface cross-cut tester, through Scotch600 adhesive tapes
Adhesion 70 times, peeling rate is less than 3.5%；Transparent performance：It can be seen that light transmission rate≤90%.
Preparation method of the invention is simple, the easy, environmental protection of safety, wide application.
Coating prepared by the present invention is particularly suited for resin lens, for the light transmittance, long-acting antifog for improving resin lens
Property has clear and definite improvement result, and can be with resin lens strong bonded.The coating can also be coated in unorganic glass, polymer sheet
Material or film, automobile sun film, the helmet etc. are needed on antifog material or product.
Brief description of the drawings
Specific embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the photo of long-acting antifog sol solutionses prepared by the embodiment of the present invention 1.
Fig. 2 shows the photo of the resin lens of the applying coating of the embodiment of the present invention 1.
Fig. 3 shows the antifog survey of the resin lens in 95% time 2h of temperature 70 C humidity of the applying coating of the embodiment of the present invention 1
Examination photo (left side is blank sample, and the right side is the sample of embodiment 1).
Fig. 4 shows the resin lens of the applying coating of the embodiment of the present invention 1, is placed 30 hours in -30 DEG C of refrigerators, takes out
The antifog test photo for shooting immediately afterwards (left side is blank sample, and the right side is the sample of embodiment 1).
Fig. 5 shows pencil (8H) cut photo of the resin lens of the applying coating of the embodiment of the present invention 1.
It is viscous through Scotch600 adhesive tapes again that Fig. 6 shows that the resin lens of the applying coating of the embodiment of the present invention 1 draw lattice through cross-cut tester
Refrigerator after attached 70 times at -30 DEG C is placed 30 hours, the photo shot immediately after taking-up (left side is blank sample).
Fig. 7 shows the UV-visible absorption spectrum of the resin lens of the applying coating of the embodiment of the present invention 1.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
The preparation method of the long-acting antifog clear coat of high intensity, step is as follows：
1) in a reservoir, PVA powder is mixed with water, is heated and is stirred in temperature is 85~100 DEG C of water-baths of temperature,
It is well mixed, it is configured to the PVA aqueous solution that mass concentration is 8wt%；
2) 5.33mL~8.48mL tetraethyl orthosilicates (TEOS) are added drop-wise to 100mL steps 1) in the PVA aqueous solution that obtains,
90min is stirred under the bath temperature of 60 DEG C of reaction temperature, the pH to 5~6 of nitre acid-conditioning solution is added, continues to stir 60min,
1.77~2.83mL 3- glycydoxy trimethoxy silanes are added after solution is transparent, wherein, tetraethyl orthosilicate
The amount ratio of material of amount and 3- glycydoxy trimethoxy silanes of material be 3:1；Stirring 60min, room temperature
Lower standing 8h, obtains long-acting antifog sol solutionses；Wherein, the amount of the material of hydroxyl contained in sol solutionses be 7.35wt%~
7.8wt%, the form of the long-acting antifog sol solutionses of gained is as shown in Figure 1；
3) resin lens that will clean 5min under 650V, 900mL/min throughputs with oxygen plasma are put into step 2)
The sol solutionses dipping 10s for obtaining, then slowly takes out, and places 4min, 20min is toasted in 160 DEG C of baking oven, then rapidly
4min is cooled down at a temperature of -15 DEG C and obtains the long-acting antifog clear coat of high intensity, such as Fig. 2 of the photo containing cated resin lens
It is shown.
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement is not hazed still for 4.5 hours, as a result as shown in Figure 3；Under the conditions of -30 DEG C freeze 30 hours, in 25 DEG C at room temperature not
Mist, as a result (in Fig. 4, English alphabet is only background, for the transparency of show layers, without other meanings as shown in Figure 4.)；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 8H, as a result as shown in Figure 5；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
Less than 3%, as a result (in Fig. 6, English alphabet is only background, for the transparency of show layers, without other meanings as shown in Figure 6
Justice.)；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region Tou Guo Shuai≤91%, as a result such as Fig. 7
It is shown.
Embodiment 2
The preparation method of the long-acting antifog clear coat of high intensity, step is as follows：
1) in a reservoir, PVA powder is mixed with water, is heated and is stirred in temperature is 85~100 DEG C of water-baths of temperature,
It is well mixed, it is configured to the PVA aqueous solution that mass concentration is 12wt%；
2) 10.3mL~16.5mL tetraethyl orthosilicates are added drop-wise to 100mL steps 1) in the PVA aqueous solution that obtains, in reaction
80min is stirred under the bath temperature that 65 DEG C of temperature, the pH for adding nitre acid-conditioning solution is 3~4, proceed to stir 70min, treated
11.64~18.65mL3- glycydoxy trimethoxy silanes are added after solution is transparent, wherein, tetraethyl orthosilicate
The amount ratio of material of amount and 3- glycydoxy trimethoxy silanes of material be 1:1；Stirring 45min, room temperature
Lower standing 6h, obtains long-acting antifog sol solutionses；The amount of the material of hydroxyl wherein contained in sol solutionses be 5.45wt%~
5.65wt%.
3) resin lens that will clean 8min under 700V, 1000mL/min throughputs with oxygen plasma are put into step 2)
The sol solutionses dipping 20s for obtaining, then slowly takes out, and places 5min, 12min is toasted in 170 DEG C of baking oven, then rapidly
6min is cooled down at -10 DEG C and obtains the long-acting antifog clear coat of high intensity.
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement is not hazed still for 5 hours；Freezed 30 hours under the conditions of -30 DEG C, do not hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 9H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
Less than 3.2%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.7%.
Embodiment 3
The preparation method of the long-acting antifog clear coat of high intensity, step is as follows：
1) in a reservoir, PVA powder is mixed with water, is heated and is stirred in temperature is 85~100 DEG C of water-baths of temperature,
It is well mixed, it is configured to the PVA aqueous solution that mass concentration is 20wt%；
2) 3.13mL~3.65mL tetraethyl orthosilicates are added drop-wise to 100mL steps 1) in the PVA aqueous solution that obtains, in reaction
70min is stirred under the bath temperature of temperature 70 C, the pH for adding nitre acid-conditioning solution is 1~5, proceed to stir 80min, treated
10.67~12.83mL 3- glycydoxy trimethoxy silanes are added after solution is transparent, wherein, tetraethyl orthosilicate
The amount ratio of material of amount and 3- glycydoxy trimethoxy silanes of material be 1:3；Stirring 50min, room temperature
Lower standing 12h, obtains long-acting antifog sol solutionses；The amount of the material of hydroxyl wherein contained in sol solutionses be 4.8wt%~
4.85wt%；
3) resin lens that will be cleaned 5 minutes under 650V, 800mL/min throughputs with oxygen plasma are put into step 2)
The sol solutionses dipping 25s for obtaining, then slowly takes out, and places 8min, 10min is toasted in 160 DEG C of baking oven, then rapidly
10min is cooled down at -5 DEG C and obtains the long-acting antifog clear coat of high intensity.
Anti-fog performance is tested：In temperature it is the environment that 50 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement is not hazed still for 4.8 hours；Freezed 30 hours under the conditions of -30 DEG C, do not hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 8H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
Less than 2.5%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.8%.
Embodiment 4
Repeat embodiment 1, difference is, by step 3) in chilling temperature be changed to 10 DEG C, remaining condition is constant, is prepared into
To the long-acting antifog clear coat of high intensity.
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement is not hazed still for 4.2 hours；Freezed 30 hours under the conditions of -20 DEG C, do not hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 8H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
Less than 3.5%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.3%.
Embodiment 5
Embodiment 1 is repeated, difference is that nitric acid is changed to the one kind in hydrochloric acid, sulfuric acid and phosphoric acid respectively, and remaining condition is not
Become, obtain the long-acting antifog clear coat of high intensity, performance is close with embodiment 1.
Embodiment 6
Embodiment 1 is repeated, difference is that PVA is changed to the one kind in polycarboxylic acids, polyureas respectively, and remaining condition is constant, obtains
To the long-acting antifog clear coat of high intensity, performance is close with embodiment 1.
Embodiment 7
Embodiment 1 is repeated, difference is that 3- glycydoxy trimethoxy silanes are changed into aminopropyl respectively
Triethoxysilane, γ-aminopropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy silane, vinyl three
Ethoxysilane, vinyltrimethoxy silane, ('beta '-methoxy ethyoxyl) silane of vinyl three and N- (β-aminoethyl)-γ-
The mixing of one or more in aminopropyl triethoxysilane, remaining condition is constant, obtains the long-acting antifog transparent painting of high intensity
Layer, performance is close with embodiment 1.
Comparative example 1
Repeat embodiment 1, difference is, by step 3) in the temperature toasted in an oven be changed to 150 DEG C, remaining condition is not
Become, prepare clear coat.Test result is as follows：
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement can haze；95min is freezed under the conditions of -30 DEG C, starts to haze at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 6H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
Up to 8.5%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.7%.
Comparative example 2
Repeat embodiment 1, difference is, by step 3) in the temperature toasted in an oven be changed to 215 DEG C, remaining condition is not
Become, prepare clear coat.Test result is as follows：
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement can haze；95min is freezed under the conditions of -30 DEG C, is hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 6H,；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
It is 7.2%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region Tou Guo Shuai≤90.7%.
Comparative example 3
Repeat embodiment 1, difference is, by step 3) in chilling temperature be changed to 20 DEG C, remaining condition is constant, is prepared into
To the long-acting antifog clear coat of high intensity.
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement can haze；65min is freezed under the conditions of -30 DEG C, is hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 5H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
It is 6.5%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.5%.
Comparative example 4
Repeat embodiment 1, difference is, by step 2) in bath temperature be changed to 90 DEG C, remaining condition is constant, is prepared into
To the long-acting antifog clear coat of high intensity.
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement can haze；65min is freezed under the conditions of -30 DEG C, is hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 6H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
It is 6.8%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.6%.
Comparative example 5
Repeat embodiment 1, difference is, by step 2) in " by 5.33mL~8.48mL tetraethyl orthosilicates (TEOS) drop
It is added to 100mL steps 1) in the PVA aqueous solution that obtains " be changed to " by 5.33mL~8.48mL tetraethyl orthosilicates (TEOS) and ethanol
(mass ratio is 1:3) mixed liquor is added drop-wise to 100mL steps 1) in the PVA aqueous solution that obtains ", remaining condition is constant, is prepared into
To the long-acting antifog clear coat of high intensity.
Anti-fog performance is tested：In temperature it is the environment that 70 DEG C of humidity is 95% by the long-acting antifog clear coat of gained high intensity
Lower placement can haze；Freezed 15 hours under the conditions of -30 DEG C, hazed at room temperature in 25 DEG C；
Strength character is tested：Tested using pencil hardness method, strength of coating reaches 6H；
Firmness is tested：Hundred lattice are marked in coating surface cross-cut tester, is adhered to 70 times through Scotch600 adhesive tapes, peeling rate
It is 5.6%；
Transparency test：Tested through ultraviolet-visible spectrophotometer, it is seen that light region transmitance 90.9%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not right
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all of implementation method cannot be exhaustive here, it is every to belong to this hair
Obvious change that bright technical scheme is extended out changes row still in protection scope of the present invention.
Claims (10)
1. the preparation method of the long-acting antifog clear coat of high intensity, it is characterised in that the preparation method comprises the following steps：
1) polymer powder that main chain or side chain are contained into hydrophilic radical mixes with water, and it is 5%~25% to be configured to mass concentration
Aqueous solutions of polymers；
2) by step 1) aqueous solutions of polymers that obtains stirs 30~720min under the bath temperature that temperature is 10~70 DEG C, plus
Enter organosilane reagents, add inorganic acid, regulation pH value of solution to 1~7 continues to stir 30~720min, after solution is transparent
Organo silane coupling agent is added, stirring stands at room temperature, obtains long-acting antifog sol solutionses；
3) resin lens are placed in step 2) in the long-acting antifog sol solutionses that obtain, impregnate 5~120s, then slowly take out,
2~10min is placed, is dried in an oven, then cool down 2~10min at a temperature of -20~15 DEG C rapidly, obtain high intensity long-acting
Antifog clear coat；Wherein, the temperature of drying is 160~200 DEG C, and the time of drying is 2~240min.
2. preparation method according to claim 1, it is characterised in that the main chain or side chain contain the polymerization of hydrophilic radical
Hydrophilic radical is amino, urea groups, sulfydryl, hydroxyl, azanol base, carboxyl or ester group in thing；Preferably, the main chain or side chain contain
The polymer of hydrophilic radical be selected from amino polymer, polyureas, sulfydryl polymer, polyvinyl alcohol, polymeric hydroxylamine, polyethylene glycol,
One or more in polycarboxylic acids, polyvinyl acetate, polyethyleneglycol block copolymer.
3. preparation method according to claim 1, it is characterised in that step 2) in, organosilane reagents and organosilan
The addition of coupling agent, is according to step 1) described in main chain or side chain contain the thing of hydrophilic radical in the polymer of hydrophilic radical
The amount of matter is 5 with the ratio of the amount of the material of organosilane reagents:1~1:0, described main chain or side chain contains the poly- of hydrophilic radical
The amount of the material of hydrophilic radical and the ratio of the amount of the material of organo silane coupling agent are 20 in compound:1~1:20.
4. preparation method according to claim 1, it is characterised in that step 2) in, organosilane reagents and organosilan
The addition of coupling agent, is according to step 1) described in main chain or side chain contain the thing of hydrophilic radical in the polymer of hydrophilic radical
The amount of matter is 5 with the ratio of described organosilane reagents and the amount of total material of organo silane coupling agent:1~20:1.
5. preparation method according to claim 1, it is characterised in that step 3) in, the temperature of the cooling is -20~0
DEG C, cool time is 2~5min.
6. preparation method according to claim 1, it is characterised in that the temperature of the drying is 180~190 DEG C, drying
Time be 5~60min.
7. preparation method according to claim 1, it is characterised in that the organosilane reagents are selected from 3- aminopropyls three
Ethoxysilane, 3- Mercaptopropyltriethoxysilanes, MTMS, tetramethoxy-silicane, tetraethyl orthosilicate, just
One or more in silicic acid propyl ester and positive isopropyl silicate；The organo silane coupling agent is selected from γ-aminopropyl trimethoxy
Silane, aminopropyl triethoxysilane, 3- glycydoxies trimethoxy silane, γ-methacryloxy third
Base trimethoxy silane, VTES, vinyltrimethoxy silane, vinyl three ('beta '-methoxy ethyoxyl)
One or more in silane and N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane.
8. preparation method according to claim 1, it is characterised in that the inorganic acid is selected from hydrochloric acid, sulfuric acid, nitric acid and phosphorus
One or more in acid.
9. preparation method according to claim 1, it is characterised in that step 3) in, the resin lens before dipping, first
Resin lens are pre-processed, the method for pretreatment is：With oxygen plasma in 600~800V, 800~1200mL/min leads to
5~10min is cleaned under tolerance.
10. the long-acting antifog clear coat of high intensity that the preparation method as described in any one of claim 1~9 is prepared is in tree
Application in fat eyeglass.
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| CN107903734A (en) * | 2017-11-28 | 2018-04-13 | 张晓婕 | The preparation method of water-fast long-acting antifog frost-resistant high transparency coating with self-healing properties |
| CN109180983A (en) * | 2018-09-25 | 2019-01-11 | 江南大学 | A kind of long-acting anti-fog and antifrost film and preparation method thereof |
| CN109836918A (en) * | 2019-02-26 | 2019-06-04 | 合肥酷飞新材料科技有限公司 | A kind of anti-fogging liquid and preparation method thereof |
| CN112110654A (en) * | 2020-09-25 | 2020-12-22 | 常州大学 | Preparation method and application of optical anti-reflection antifogging film |
| CN115627089A (en) * | 2022-10-16 | 2023-01-20 | 杭州梵因科技有限公司 | Preparation method of high-efficiency cold fog antifogging agent for lenses |
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| CN112110654B (en) * | 2020-09-25 | 2022-07-05 | 常州大学 | Preparation method and application of optical anti-reflection antifogging film |
| CN115627089A (en) * | 2022-10-16 | 2023-01-20 | 杭州梵因科技有限公司 | Preparation method of high-efficiency cold fog antifogging agent for lenses |
| CN115627089B (en) * | 2022-10-16 | 2023-06-09 | 杭州梵因科技有限公司 | Preparation method of efficient cold fog antifogging agent for lenses |
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