CN117164247A - Nanometer optical glass with antifouling property and preparation method thereof - Google Patents
Nanometer optical glass with antifouling property and preparation method thereof Download PDFInfo
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- CN117164247A CN117164247A CN202311014310.4A CN202311014310A CN117164247A CN 117164247 A CN117164247 A CN 117164247A CN 202311014310 A CN202311014310 A CN 202311014310A CN 117164247 A CN117164247 A CN 117164247A
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- 239000005304 optical glass Substances 0.000 title claims abstract description 58
- 230000003373 anti-fouling effect Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 179
- 239000002131 composite material Substances 0.000 claims abstract description 126
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 51
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011521 glass Substances 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 229920001661 Chitosan Polymers 0.000 claims abstract description 18
- 239000011258 core-shell material Substances 0.000 claims abstract description 4
- 239000011858 nanopowder Substances 0.000 claims abstract description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 63
- 239000002002 slurry Substances 0.000 claims description 58
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 57
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 26
- 239000011248 coating agent Substances 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 24
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 17
- 239000003822 epoxy resin Substances 0.000 claims description 16
- 229920000647 polyepoxide Polymers 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 15
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims description 15
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 15
- 229910021389 graphene Inorganic materials 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910002651 NO3 Inorganic materials 0.000 claims description 14
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000003999 initiator Substances 0.000 claims description 7
- 239000004005 microsphere Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 9
- 230000007774 longterm Effects 0.000 abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 229910010413 TiO 2 Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Paints Or Removers (AREA)
- Surface Treatment Of Glass (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of optical glass, in particular to nano optical glass with an antifouling property, which comprises a glass substrate, and a first TiO2 composite layer, a nano antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate; the first TiO2 composite layer and the second TiO2 composite layer both comprise TiO2-PS core-shell structure nano powder, and the nano antibacterial composite layer comprises modified lanthanum oxide and chitosan. The optical glass prepared by the invention has good light transmittance, good long-term antibacterial effect, good antifouling performance and better comprehensive performance of products.
Description
Technical Field
The invention relates to the technical field of optical glass, in particular to nano optical glass with an antifouling property and a preparation method thereof.
Background
The application range of the glass material is wide, wherein the optical glass is glass capable of changing the propagation direction of light, and the narrow optical glass refers to colorless optical glass; the broad sense of optical glass also includes colored optical glass, quartz optical glass, and the like. With the development of the age, the demand for optical glass is increasing, and the demand for optical glass is also increasing. In the prior art, more research and development are carried out on optical glass, for example, chinese scratch with publication number of CN 114735944A discloses optical glass with nano-material coated on the surface and a preparation method thereof, wherein a layer of nano-composite slurry and a layer of modified titanium dioxide slurry are sequentially coated on the glass, so that the obtained optical glass has high refractive index and stronger acid-base resistance, wear resistance and corrosion resistance. However, in practical application, the optical glass prepared by the technology is still not ideal in light transmittance, anti-fouling property and antibacterial property, and needs further improvement.
Disclosure of Invention
The technical problem solved by the invention is to provide the nano optical glass with better antifouling property, light transmittance and antibacterial property so as to better meet the practical application.
The second technical problem to be solved by the invention is to provide a preparation method of the nano optical glass with the antifouling property.
To solve the problems in the background art described above.
The technical problems solved by the invention are realized by adopting the following technical scheme:
a nanometer optical glass with antifouling property comprises a glass substrate, and a first TiO2 composite layer, a nanometer antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate; the first TiO2 composite layer and the second TiO2 composite layer both comprise TiO2-PS core-shell structure nano powder, and the nano antibacterial composite layer comprises modified lanthanum oxide and chitosan.
Further, the first TiO2 composite layer and the second TiO2 composite layer are consistent in structure and comprise the following raw materials in parts by weight: 10-12 parts of gamma-methyl propenoxy trimethoxy propyl silane, 0.7-1 part of tetrabutyl titanate and 90-110 parts of styrene.
Further, the nano antibacterial composite layer comprises the following raw materials in parts by weight: 10-20 parts of cyanate resin, 2-5 parts of epoxy resin, 10-20 parts of modified lanthanum oxide, 5-8 parts of dibutyl tin dilaurate, 5-10 parts of styrene, 10-20 parts of acetone, 5-15 parts of graphene, 0.2-0.5 part of chitosan and 0.1-0.4 part of nitrate.
A preparation method of nano optical glass with antifouling property comprises the following steps:
preparing TiO2 composite slurry:
preparing nano antibacterial composite slurry:
and coating the TiO2 composite slurry on the surface of the glass substrate to form a first TiO2 composite layer, coating the nano antibacterial composite slurry to form a nano antibacterial composite layer, and continuing coating the TiO2 composite slurry to form a second TiO2 composite layer.
Further, the method for preparing the TiO2 composite slurry comprises the following steps: modification of colloidal TiO from tetrabutyl titanate hydrolysis with gamma-methacryloxytrimethoxypropylsilane 2 Preparing MPS-TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Then MPS-TiO 2 TiO is prepared by in-situ polymerization method for styrene 2 And (3) compounding the sizing agent.
Further, tiO is prepared 2 The method for the composite sizing agent comprises the following steps: tetrabutyl titanate and gamma-methyl propylene oxy trimethoxy propyl silane are mixed and N-N' dimethylformamide is used as solvent, and MPS-TiO is obtained through stirring reaction 2 Washing gel liquid and MPS-TiO2 gel, and drying to obtain MPS-TiO 2 A powder; MPS-TiO 2 Dissolving the powder in N-N' dimethylformamide, carrying out ultrasonic treatment for 25-30 min, then adding styrene, and dropwise adding an initiator under the condition of introducing nitrogen to react, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
Further, the method for preparing the nano antibacterial composite slurry comprises the following steps: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene, chitosan and nitrate, reacting for 10-20 s, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
The beneficial effects are that: the nano optical glass with the antifouling property is prepared by sequentially coating a glass substrate with the nano optical glassSecondary coating of first TiO 2 Composite layer, nano antibacterial composite layer and second TiO 2 Composite layers, wherein the unique TiO 2 PS core-shell structure nano powder material and double-layer TiO 2 The composite layer is arranged, so that the transmittance of light is effectively increased, ultraviolet rays are more fully filtered and absorbed, and better photochemical reaction can be generated, so that the antifouling property and the self-cleaning property of the optical glass are enhanced. In addition, in the nano antibacterial composite layer, gamma-mercaptopropyl trimethoxy silane is grafted on the surface of nano lanthanum oxide and chitosan is combined, so that the nano lanthanum oxide and other components are fully crosslinked, the coating is more closely connected, the crosslinking degree is higher, the refractive index is further improved, in addition, the addition of the chitosan is favorable for fully dispersing nano lanthanum oxide particles and silver ions, agglomeration among ions is prevented, and the release of antibacterial ions is prevented from being too fast, so that the nano optical glass has a long-term slow-release antibacterial effect.
According to the preparation method of the nano optical glass with the antifouling property, the prepared nano optical glass has the advantages of good light transmittance, strong ultraviolet resistance, good antifouling effect, long-term slow-release antibacterial effect, simple preparation process, completion through relatively simple wet coating and suitability for mass production and application.
Detailed Description
In order that the manner in which the invention is attained, as well as the features and advantages thereof, will be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
Example 1
The nano optical glass with the antifouling property comprises a glass substrate, and a first TiO2 composite layer, a nano antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate.
The first TiO2 composite layer and the second TiO2 composite layer are consistent in structure and comprise the following raw materials in parts by weight: 10 parts of gamma-methacryloxy trimethoxy propyl silane, 0.8 part of tetrabutyl titanate and 100 parts of styrene.
Further, the nano antibacterial composite layer comprises the following raw materials in parts by weight: 16 parts of cyanate resin, 4 parts of epoxy resin, 12 parts of modified lanthanum oxide, 6 parts of dibutyl tin dilaurate, 6 parts of styrene, 12 parts of acetone, 8 parts of graphene, 0.4 part of chitosan and 0.3 part of nitrate.
The preparation method of the nano optical glass with the antifouling property comprises the following steps:
preparing TiO2 composite slurry: mixing tetrabutyl titanate with gamma-methacryloxy trimethoxy propyl silane, adding the mixture into a beaker, stirring and reacting for 3 hours at normal temperature by using N-N 'dimethylformamide as a solvent, then adding a proper amount of deionized water and hydrochloric acid, stirring and reacting for 5 hours at a constant temperature of 65 ℃ to obtain MPS-TiO2 gel liquid, washing the MPS-TiO2 gel with N-N' dimethylformamide, centrifuging, and then drying to obtain MPS-TiO2 powder; dissolving MPS-TiO2 powder in N-N' dimethylformamide, performing ultrasonic treatment for 30min, then adding styrene and nitrogen at 45 ℃ and dropwise adding an initiator to react, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
Preparing nano antibacterial composite slurry: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene, chitosan and nitrate, reacting for 20 seconds, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
And coating the TiO2 composite slurry on the surface of the glass substrate to form a first TiO2 composite layer, coating the nano antibacterial composite slurry to form a nano antibacterial composite layer, and continuing coating the TiO2 composite slurry to form a second TiO2 composite layer.
Example 2
The nano optical glass with the antifouling property comprises a glass substrate, and a first TiO2 composite layer, a nano antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate.
The first TiO2 composite layer and the second TiO2 composite layer are consistent in structure and comprise the following raw materials in parts by weight: 12 parts of gamma-methacryloxy trimethoxy propyl silane, 0.7 part of tetrabutyl titanate and 105 parts of styrene.
Further, the nano antibacterial composite layer comprises the following raw materials in parts by weight: 12 parts of cyanate resin, 5 parts of epoxy resin, 15 parts of modified lanthanum oxide, 8 parts of dibutyl tin dilaurate, 10 parts of styrene, 20 parts of acetone, 5 parts of graphene, 0.5 part of chitosan and 0.2 part of nitrate.
The preparation method of the nano optical glass with the antifouling property comprises the following steps:
preparing TiO2 composite slurry: mixing tetrabutyl titanate with gamma-methacryloxy trimethoxy propyl silane, adding the mixture into a beaker, stirring and reacting for 3 hours at normal temperature by using N-N 'dimethylformamide as a solvent, then adding a proper amount of deionized water and hydrochloric acid, stirring and reacting for 6 hours at a constant temperature of 60 ℃ to obtain MPS-TiO2 gel liquid, washing the MPS-TiO2 gel with N-N' dimethylformamide, centrifuging, and then drying to obtain MPS-TiO2 powder; dissolving MPS-TiO2 powder in N-N' dimethylformamide, performing ultrasonic treatment for 30min, then adding styrene, introducing nitrogen at 45 ℃ and dropwise adding an initiator for reaction, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
Preparing nano antibacterial composite slurry: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene, chitosan and nitrate, reacting for 15 seconds, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
Comparative example 1
The nano optical glass with the antifouling property comprises a glass substrate, and a nano antibacterial composite layer and a first TiO2 composite layer which are arranged on the glass substrate.
The first TiO2 composite layer comprises the following raw materials in parts by weight: 10 parts of gamma-methacryloxy trimethoxy propyl silane, 0.8 part of tetrabutyl titanate and 100 parts of styrene.
Further, the nano antibacterial composite layer comprises the following raw materials in parts by weight: 16 parts of cyanate resin, 4 parts of epoxy resin, 12 parts of modified lanthanum oxide, 6 parts of dibutyl tin dilaurate, 6 parts of styrene, 12 parts of acetone, 8 parts of graphene, 0.4 part of chitosan and 0.3 part of nitrate.
The preparation method of the nano optical glass with the antifouling property comprises the following steps:
preparing TiO2 composite slurry: mixing tetrabutyl titanate with gamma-methacryloxy trimethoxy propyl silane, adding the mixture into a beaker, stirring and reacting for 3 hours at normal temperature by using N-N 'dimethylformamide as a solvent, then adding a proper amount of deionized water and hydrochloric acid, stirring and reacting for 5 hours at a constant temperature of 65 ℃ to obtain MPS-TiO2 gel liquid, washing the MPS-TiO2 gel with N-N' dimethylformamide, centrifuging, and then drying to obtain MPS-TiO2 powder; dissolving MPS-TiO2 powder in N-N' dimethylformamide, performing ultrasonic treatment for 30min, then adding styrene, introducing nitrogen at 45 ℃ and dropwise adding an initiator for reaction, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
Preparing nano antibacterial composite slurry: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene, chitosan and nitrate, reacting for 20 seconds, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
Coating nano antibacterial composite slurry on the surface of a glass substrate to form a nano antibacterial composite layer, and coating TiO2 composite slurry to form a first TiO2 composite layer.
Comparison document 2
The nano optical glass with the antifouling property comprises a glass substrate, and a first TiO2 composite layer, a nano antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate.
The first TiO2 composite layer and the second TiO2 composite layer are consistent in structure and comprise the following raw materials in parts by weight: 10 parts of gamma-methacryloxy trimethoxy propyl silane, 0.8 part of tetrabutyl titanate and 100 parts of styrene.
Further, the nano antibacterial composite layer comprises the following raw materials in parts by weight: 16 parts of cyanate resin, 4 parts of epoxy resin, 12 parts of modified lanthanum oxide, 6 parts of dibutyltin dilaurate, 6 parts of styrene, 12 parts of acetone, 8 parts of graphene and 0.3 part of nitrate.
The preparation method of the nano optical glass with the antifouling property comprises the following steps:
preparing TiO2 composite slurry: mixing tetrabutyl titanate with gamma-methacryloxy trimethoxy propyl silane, adding the mixture into a beaker, stirring and reacting for 3 hours at normal temperature by using N-N 'dimethylformamide as a solvent, then adding a proper amount of deionized water and hydrochloric acid, stirring and reacting for 5 hours at a constant temperature of 65 ℃ to obtain MPS-TiO2 gel liquid, washing the MPS-TiO2 gel with N-N' dimethylformamide, centrifuging, and then drying to obtain MPS-TiO2 powder; dissolving MPS-TiO2 powder in N-N' dimethylformamide, performing ultrasonic treatment for 30min, then adding styrene, introducing nitrogen at 45 ℃ and dropwise adding an initiator for reaction, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
Preparing nano antibacterial composite slurry: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene and nitrate, reacting for 20s, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
And coating the TiO2 composite slurry on the surface of the glass substrate to form a first TiO2 composite layer, coating the nano antibacterial composite slurry to form a nano antibacterial composite layer, and continuing coating the TiO2 composite slurry to form a second TiO2 composite layer.
Comparative example 3
The nano optical glass with the antifouling property comprises a glass substrate, and a first TiO2 composite layer, a nano antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate.
The first TiO2 composite layer and the second TiO2 composite layer are consistent in structure and comprise the following raw materials in parts by weight: 10 parts of gamma-methacryloxy trimethoxy propyl silane, 0.8 part of tetrabutyl titanate and 100 parts of styrene.
Further, the nano antibacterial composite layer comprises the following raw materials in parts by weight: 16 parts of cyanate resin, 4 parts of epoxy resin, 12 parts of modified lanthanum oxide, 6 parts of dibutyl tin dilaurate, 6 parts of styrene, 12 parts of acetone, 8 parts of graphene, 2 parts of chitosan and 0.3 part of nitrate.
The preparation method of the nano optical glass with the antifouling property comprises the following steps:
preparing TiO2 composite slurry: mixing tetrabutyl titanate with gamma-methacryloxy trimethoxy propyl silane, adding the mixture into a beaker, stirring and reacting for 3 hours at normal temperature by using N-N 'dimethylformamide as a solvent, then adding a proper amount of deionized water and hydrochloric acid, stirring and reacting for 5 hours at a constant temperature of 65 ℃ to obtain MPS-TiO2 gel liquid, washing the MPS-TiO2 gel with N-N' dimethylformamide, centrifuging, and then drying to obtain MPS-TiO2 powder; dissolving MPS-TiO2 powder in N-N' dimethylformamide, performing ultrasonic treatment for 30min, then adding styrene, introducing nitrogen at 45 ℃ and dropwise adding an initiator for reaction, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
Preparing nano antibacterial composite slurry: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene, chitosan and nitrate, reacting for 20 seconds, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
And coating the TiO2 composite slurry on the surface of the glass substrate to form a first TiO2 composite layer, coating the nano antibacterial composite slurry to form a nano antibacterial composite layer, and continuing coating the TiO2 composite slurry to form a second TiO2 composite layer.
Comparative example 4
In this comparative example, the method for producing an optical glass comprises the steps of:
s1: preparation of nanocomposite slurry: a: adjusting the pH of 10 parts of acetone solution to 4.5 by using 0.5 part of acetic acid, adding 0.1 part of gamma-mercaptopropyl trimethoxy silane after uniformly mixing, adding 30 parts of nano lanthanum oxide, reacting for 10s, performing ultrasonic reaction for 0.5h, and filtering to obtain pretreated lanthanum oxide; b: uniformly mixing 2 parts of dimethyl sulfoxide, 0.1 part of azodiisobutyronitrile, 1 part of alpha-methylpyridine and 1 part of tetraethoxysilane, adding 5 parts of pretreated lanthanum oxide, carrying out ultrasonic treatment for 10min, slowly dropwise adding 5 parts of methyl methacrylate, reacting for 1h, cooling, carrying out suction filtration, washing with absolute ethyl alcohol and water, carrying out vacuum drying, and filtering to obtain modified lanthanum oxide; c: uniformly mixing 10 parts of dried cyanate resin with 2 parts of epoxy resin, adding 5 parts of dibutyltin dilaurate, dispersing for 10s, adding 5 parts of pretreated styrene monomer, 10 parts of modified lanthanum oxide and 5 parts of graphene, reacting for 10s, adding 10 parts of acetone solution, and uniformly mixing to obtain the epoxy resin;
s2: preparation of modified titanium dioxide slurry: dissolving 20 parts of tetrabutyl titanate in 15 parts of absolute ethyl alcohol, adding 5 parts of glacial acetic acid, uniformly mixing to obtain a solution A, dissolving 3 parts of cobalt chloride hexahydrate, 4 parts of urea and 4 parts of thiourea in 10 parts of absolute ethyl alcohol, uniformly mixing, performing ultrasonic treatment for 5min to obtain a solution B, slowly adding the solution B into the solution A, reacting for 1h, standing for 5h, evaporating the solvent at 70 ℃, drying, adding 10 parts of sodium dodecyl sulfate, reacting for 5min, adding 5 parts of water, and reacting for 15min to obtain modified titanium dioxide slurry;
s3: melting and clarifying 5 parts of silicon dioxide, 10 parts of diboron trioxide, 60 parts of bismuth oxide, 0.5 part of barium oxide, 0.5 part of antimonous oxide, 5 parts of zinc oxide and 10 parts of cerium oxide at 700 ℃, pouring into a preheating mould, and annealing at 300 ℃;
s4: coating a layer of nano composite slurry on the outer surface of the optical glass, and then coating a layer of modified titanium dioxide slurry to form a titanium dioxide layer, thus obtaining the optical glass.
In the step S1, the step of pretreatment of the styrene monomer is as follows: styrene monomer should be mixed with sodium hydroxide, ultrasonically reacted for 10-20min, the upper organic phase is reserved, washed with water, and dried with anhydrous calcium chloride.
The optical glasses prepared in examples 1 to 2 and comparative examples 1 to 4 were subjected to performance test, and the test results are shown in table 1.
Transmittance: the average transmittance of light with a wavelength of 355nm to 1035nm was measured by taking each optical glass.
Bacteriostasis: the optical glass is soaked in the methyl orange solution, an ultraviolet lamp and a visible light source lamp are used for irradiation for 6 hours at the same time, the absorbance of the methyl orange solution before and after illumination is measured, and the methyl orange degradation rate is calculated.
Table 1 comparison of properties of optical glass
As can be seen from Table 1, after the technical scheme of the invention is applied, the optical glass can have higher refractive index, good anti-reflection effect is achieved, the light transmittance of the optical glass can reach more than 95%, the antibacterial performance is good, and the antibacterial components in the coating can be slowly and uniformly released, so that a long-term good antibacterial effect is achieved. It is apparent from the combination of examples 1 and 2, and comparative examples 2 and 3 that the addition of a proper amount of chitosan can not only achieve a better antibacterial sustained-release effect, but also improve the light transmittance to some extent.
The optical glasses prepared in examples 1-2 and comparative example 4 were exposed to air for one month under the same conditions in terms of anti-fouling performance, and the optical glasses of example 1 and example 2 were observed to have significantly better surface cleanliness than the optical glass prepared in comparative example 4, which indicates that the optical glass prepared in the technical scheme of the present invention has better self-cleaning property.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The nanometer optical glass with the antifouling property is characterized by comprising a glass substrate, and a first TiO2 composite layer, a nanometer antibacterial composite layer and a second TiO2 composite layer which are arranged on the glass substrate; the first TiO2 composite layer and the second TiO2 composite layer both comprise TiO2-PS core-shell structure nano powder, and the nano antibacterial composite layer comprises modified lanthanum oxide and chitosan.
2. The nano optical glass with the antifouling property according to claim 1, wherein the first TiO2 composite layer and the second TiO2 composite layer are consistent in structure and comprise the following raw materials in parts by weight: 10 to 12 parts of gamma-methyl propylene oxy trimethoxy propyl silane, 0.7 to 1 part of TBT tetrabutyl titanate and 90 to 110 parts of styrene.
3. The nano optical glass with the antifouling property according to claim 1, wherein the nano antibacterial composite layer comprises the following raw materials in parts by weight: 10-20 parts of cyanate resin, 2-5 parts of epoxy resin, 10-20 parts of modified lanthanum oxide, 5-8 parts of dibutyl tin dilaurate, 5-10 parts of styrene, 10-20 parts of acetone, 5-15 parts of graphene, 0.2-0.5 part of chitosan and 0.1-0.4 part of nitrate.
4. The preparation method of the nano optical glass with the antifouling property is characterized by comprising the following steps:
preparing TiO2 composite slurry:
preparing nano antibacterial composite slurry:
and coating the TiO2 composite slurry on the surface of the glass substrate to form a first TiO2 composite layer, coating the nano antibacterial composite slurry to form a nano antibacterial composite layer, and continuing coating the TiO2 composite slurry to form a second TiO2 composite layer.
5. The method for preparing nano optical glass with antifouling property according to claim 4, wherein the method for preparing the TiO2 composite slurry comprises the following steps: modifying colloidal TiO2 obtained by tetrabutyl titanate hydrolysis by gamma-methacryloxytrimethoxypropylsilane to prepare MPS-TiO2; and then preparing the MPS-TiO2 and styrene into the TiO2 composite slurry by an in-situ polymerization method.
6. The method for preparing a nano optical glass with anti-fouling property according to claim 5, wherein the method for preparing the TiO2 composite slurry comprises the following steps: mixing tetrabutyl titanate and gamma-methacryloxy trimethoxy propyl silane, using N-N' dimethylformamide as a solvent, stirring and reacting to obtain MPS-TiO2 gel liquid, washing the MPS-TiO2 gel, and drying to obtain MPS-TiO2 powder; dissolving MPS-TiO2 powder in N-N' dimethylformamide, performing ultrasonic treatment for 25-30 min, then adding styrene, and dropwise adding an initiator under the condition of introducing nitrogen to react, wherein the obtained microsphere dispersion liquid is TiO2 composite slurry.
7. The method for preparing nano optical glass with antifouling property according to claim 4, wherein the method for preparing nano antibacterial composite slurry comprises the following steps: and (3) uniformly mixing cyanate resin, epoxy resin and dibutyltin dilaurate, continuously adding styrene, modified lanthanum oxide, graphene, chitosan and nitrate, reacting for 10-20 s, adding an acetone solution, and uniformly mixing to obtain the nano lanthanum oxide composite slurry.
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