CN1237113C - Light scattering material of organic glass modified by Nano silicon in use for lighting and displaying, and preparation method - Google Patents
Light scattering material of organic glass modified by Nano silicon in use for lighting and displaying, and preparation method Download PDFInfo
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- CN1237113C CN1237113C CN 03127636 CN03127636A CN1237113C CN 1237113 C CN1237113 C CN 1237113C CN 03127636 CN03127636 CN 03127636 CN 03127636 A CN03127636 A CN 03127636A CN 1237113 C CN1237113 C CN 1237113C
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- mma
- sio
- light scattering
- organic glass
- scattering material
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- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000000149 argon plasma sintering Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011521 glass Substances 0.000 title claims abstract description 10
- 239000005543 nano-size silicon particle Substances 0.000 title claims description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 6
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 22
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 12
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 239000000049 pigment Substances 0.000 claims description 3
- 241000237502 Ostreidae Species 0.000 claims description 2
- 239000004902 Softening Agent Substances 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims description 2
- 239000011858 nanopowder Substances 0.000 claims description 2
- 235000020636 oyster Nutrition 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 1
- 239000002243 precursor Substances 0.000 claims 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 150000004965 peroxy acids Chemical class 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 4
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 239000002002 slurry Substances 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 230000010355 oscillation Effects 0.000 abstract 1
- 230000000149 penetrating effect Effects 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 abstract 1
- 238000009849 vacuum degassing Methods 0.000 abstract 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 12
- 239000004926 polymethyl methacrylate Substances 0.000 description 12
- 238000002834 transmittance Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000005286 illumination Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- YZBOVSFWWNVKRJ-UHFFFAOYSA-N Monobutylphthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(O)=O YZBOVSFWWNVKRJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- 239000012986 chain transfer agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000382 optic material Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- -1 siloxane compound Chemical class 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Polymerisation Methods In General (AREA)
Abstract
The present invention provides an organic glass light scattering material modified by nanometer silicon, and a preparation method thereof. The material comprises the components of the weight percentage content: 86.0 to 98.5% of MMA, 0.1 to 30% of nanometer SiO2 powder, 0.1 to 0.3% of benzoyl salt of peroxy acid, 1.0 to 10.0% of dibutyl phthalate and 0.1 to 0.5% of antiageing agent UV-9 or 49. Firstly, the nanometer SiO2 powder is mixed into an MMA monomer by the oscillation of high frequency ultrasonic waves so that the MMA monomer is in milky transparent state; after an initiator and other components are added for vacuum degassing, all the components are prepolymerized at 90 DEG C; after the slurry is cooled and filled into a mould, the slurry is treated at 25 to 100 DEG C for 24 to 72 hours. The methOd has the advantages of simple technology and easy control, and the material has a spectrum penetrating curve approximating to body material and homogeneous light scattering distribution and can be used as the light scattering material of lighting display devices.
Description
One, affiliated technical field: the present invention relates to inorganics doped polymeric optical material and preparation thereof, belong to nano combined optical material field.
Two, background technology: inhomogeneous as polarizability in the medium when light passes through solid-state or fluid media according to the electromagnetic theory of scattering of light, will produce light scattering phenomenon.And the polarizability of material and its specific refractory power are proportional, that is to say when having the specific refractory power uneven distribution in the medium scattering of light will take place.Causing the uneven reason of specific refractory power can be the density fluctuation of medium itself, also can be to be mixed with the different particulate scatter point of specific refractory power.It is polymethylmethacrylate (PMMA) that Japanese Patent JP04 59,854 discloses a kind of matrix, and scattering object is the inorganic particles with certain grain size distribution, zinc oxide (ZnO) for example, lime carbonate (CaCO
3), the preparation method of the light diffuse-reflectance paper of zeolite etc.When set of dispense than for particle diameter be ZnO0.2 part of 0.5 μ m, particle diameter is the CaCO of 0.5 μ m
31.5 part and 100 parts PMMA carry out direct blend and prepare light-scattering material because transparency is lower, be only applicable to throw light on occasions such as direction board.
Nanometer SiO
2The doping pmma material is a kind of of the advanced composite material that grows up along with the rise of nanotechnology phase late 1980s.It also is confined to the experimental study stage at present." applied chemistry " 2002 the 9th phases have been reported the work that Zhang Qi defends etc., adopt sol-gel technique, and article thinks that the alternate intermiscibility of its organic/inorganic two is good, do not produce to be separated, and material is transparent, and transmittance can reach about 80%.Material that it is generally acknowledged such preparation only limits to the former organic glass surface of modification, strengthens the hardness and the thermotolerance of synthetic glass by coating." engineering plastics application " 1994,22 (5) 47; " macromolecular material is learned and engineering " 1999,15 (1), 108 and " functional materials " 1995,26 (6), 510 have been reported the work of relevant silicon doping, and mass polymerization, SiO are adopted in specimen preparation
2The use of surface treatment agent does not make the dispersing uniformity of nano particle that bigger improvement is arranged.Chinese patent 01115311.3 discloses " preparation nanometer SiO
2The method of modified optical plastic fibres ", the MMA monomer is 5 with the ratio of siloxane compound: 1-50: 1, add the azo class of total amount 0.1-1% or the mercaptan type chain transfer agent of peroxide initiator and 0.03-0.2%, obtain mechanical property, the nanometer SiO that optical property is improved
2The modified PMMA fiber optic materials.
Three, summary of the invention: the objective of the invention is to the optical characteristics of modified PMMA, make it become light-scattering material.By to nanometer SiO
2The control of particle size and PMMA presoma component ratio makes the light of the various wavelength of the even scattering of composite property, not only can strengthen body brightness and give good visual experience as illumination, display light scattering material.
Purpose of the present invention can reach by following measure:
A kind of preparation method of nano-silicon modified organic glass light-scattering material comprises the following steps of carrying out successively:
1, by institute at optical wavelength, each component weight percent content of adjustment in following component concentration scope, and get the raw materials ready by the prescription of adjusting;
Weight percentages of components
Methyl methacrylate MMA 86.0-98.5
Peroxy acid benzoyl BPO 0.1-0.3
Nanometer SiO
2Powder 0.1-3.0
Plasticizer phthalic acid butyl ester 1.0-10.0
Anti-aging agent UV9 or 49 0.1-0.5
2, with MMA monomer in step 1 component, take out 20% by calculating charging capacity, add the SiO that MMA calculates charging capacity 0.1-3.0% weight percent amount
2Nano powder carries out the high-frequency ultrasonic vibration and mixes, to whole SiO under 0 ℃-45 ℃
2Suspend, and MMA is creamy white, till the translucent liquid;
3, with step 2 gained liquid, with the MM mixing of other 80% weight, add the benzoyl peroxide of step 1, as the plastifying dibutyl phthalate with as ageing-resistant UV-9 or 49 as initiator, the deoxidation of mixing final vacuum is to oyster white, till the translucent liquid; With mixed solution under 90 ℃, prepolymerization in 25 minutes;
4, the prepolymer that step 3 is obtained is cooled to room temperature, and grouting is gone in the mould; 25-100 ℃ of different warm areas in water-bath, different polymerization accumulative totals down consuming time 24-72 hour.
The nanometer SiO that adds in the step 1
2The particle diameter of powder can be at 20nm between the 600nm.Also can in step 3, add the oil soluble transparent pigment, obtain colored prepolymer after the pre-polymerization.
The present invention is adulterated nanometer SiO in PMMA
2Crosslinking reaction does not take place in particle in the polymerization, nanometer SiO in the material structure
2Be dispersed in the PMMA continuum, do not change original chemical structure of fertile material and basic physical properties, nanometer SiO
2Particle is as scatter point, when its size during greater than light wavelength, forms interfering with each other of scattered light, shows various anisotropies, and conventional P MMA modification is become light-scattering material, it is generally acknowledged SiO
2And the certain physical avidity is arranged between the PMMA continuum, or claim Robert Van de Walle power.
The present invention has selected the different SiO of 20-600nm particle diameter for use
2Powder and controlled doping amount are at 0.1-3.0%, thereby control is to the scattering of light intensity of different wave length light.
Conventional P MMA and dopen Nano SiO
2The comparison of optical transmittance of PMMA, be the first-selected index that dopant material is used in optical field, provided among Fig. 1 at visible-range (400-700nm) optical transmittance rate curve, conventional P MMA is about 90%, and doping SiO
2Its spectral transmittance of the PMMA of nano particle becomes short with wavelength and slightly reduces, however this nanometer SiO just
2Particle is to the result of scattering of light, and optical wavelength is more near SiO
2Nanoparticle size, scattering are stronger.
By the mensuration of PMMA sheet material several physical parameters, as shown in table 1ly go out, conventional panels and doping plate be in density, specific refractory power, thermal expansivity, the modulus of elasticity in direct stress, both are more or less the same curved characteristic.
Several physical property measurement data of table 1
Four, the drawing of accompanying drawing explanation: Fig. 1 is the optical transmittance graphic representation, 1. is traditional synthetic glass among the figure, 2. is doping 200nm SiO
2The synthetic glass of nano particle.
Five, specific embodiment:
The preparation of the thick Si modified plate of embodiment: 20mm
Weight percentages of components
Methyl methacrylate 94.45
Benzoyl peroxide 0.15
Nanometer SiO
2Powder (200nm particle diameter) 0.2
Dibutyl phthalate 5.0
UV9 0.2
By above-mentioned ratio of components, earlier with SiO
2Powder is dispersed in the MMA monomer by the high-frequency ultrasonic vibration, add initiator, softening agent, anti-aging agent mixing then, vacuum outgas is not till have a bubble, 90 ℃ of following prepolymerizations 25 minutes, be cooled to room temperature, then this prepolymer be poured in the mould, in water-bath, press following warm area, consuming timely carry out polymerization: 25-40 ℃, 36 hours; 40-60 ℃, 20 hours; 60-70 ℃, 4 hours; 70-80 ℃, 2 hours; 80-90 ℃, 1 hour; 90-100 ℃, 0.5 hour.
Embodiment 2: Ф 45m/m bar
Weight percentages of components
Methyl methacrylate 91.05
Benzoyl peroxide 0.15
Nanometer SiO
2Powder (100nm particle diameter) 0.3
Dibutyl phthalate 8.0
UV-49 0.5
SiO
2Dispersion, deoxidation, pre-polymerization with embodiment 1 in water-bath by following warm area, consuming timely carry out polymerization: 25-30 ℃, 48 hours; 30-40 ℃, 24 hours; 40-60 ℃, 12 hours; 60-80 ℃, 12 hours; 80-90 ℃, 2 hours.
The thick red sheet material of embodiment 3:15mm
Weight percentages of components
Methyl methacrylate 98.05
Benzoyl peroxide 0.2
Nanometer SiO
2Powder (600nm particle diameter) 0.25
Dibutyl phthalate 1.0
UV-49 0.4
Red oil color 0.3
SiO
2Dispersion, deoxidation, pre-polymerization be with embodiment 1, by following warm area, consuming timely carries out polymerization: 40-50 ℃ in water-bath, 36 hours 50-60 ℃, 12 hours; 60-80 ℃, 10 hours; 80-100 ℃, 10 hours.
Embodiment 4:5mm heavy-gauge sheeting
Weight percentages of components
Methyl methacrylate 88.35
Benzoyl peroxide 0.3
Nanometer SiO
2Powder (50nm particle diameter) 2.0
Dibutyl phthalate 9.0
UV-9 0.1
The molten pigment 0.25 of transparent green oil
SiO
2Dispersion, deoxidation, pre-polymerization be with embodiment 1, by following warm area, consuming timely carries out polymerization: 45-55 ℃, 20 hours in water-bath; 55-75 ℃, 10 hours; 75-90 ℃, 5 hours.
Embodiment 5:1mm heavy-gauge sheeting
Weight percentages of components
Methyl methacrylate 86.0
Benzoyl peroxide 0.3
Nanometer SiO
2Powder (20nm particle diameter) 3.0
Dibutyl phthalate 10.0
UV-9 0.5
Blue look oil color 0.2
SiO
2Dispersion, deoxidation, pre-polymerization be with embodiment 1, by following warm area, consuming timely carries out polymerization: 50-60 ℃, 2 hours in water-bath; 60-85 ℃, 12 hours.
Claims (3)
1, a kind of preparation method of nano-silicon modified organic glass light-scattering material is characterized in that may further comprise the steps successively:
Step 1: by institute at optical wavelength, each component weight percent content of adjustment in following component concentration scope, and get the raw materials ready by the prescription of adjusting:
Weight percentages of components
Methyl methacrylate MMA 86.0-98.5
Benzoyl peroxide 0.1-0.3
Nanometer SiO
2Powder 0.1-3.0
Plasticizer phthalic acid dibutylester 1.0-10.0
Anti-aging agent UV9 or 49 0.1-0.5
Step 2: with MMA monomer in the step 1 component, take out 20%, add the SiO that MMA calculates charging capacity 0.1-3.0% weight percent amount by calculating charging capacity
2Nano powder carries out the high-frequency ultrasonic vibration and mixes, to whole SiO under 0 ℃-45 ℃
2Suspend, and MMA is creamy white, till the translucent liquid;
Step 3: with step 2 gained liquid, with the MMA mixing of other 80% weight, add the benzoyl peroxide of step 1, as the dibutyl phthalate of softening agent with as ageing-resistant UV-9 or 49 mixings as initiator, vacuum deaeration is to oyster white, till the translucent liquid;
Step 4: with the precursor that step 3 obtains, under 90 ℃, prepolymerization 25 minutes is cooled to room temperature;
Step 5: the polymers that gives that step 4 is obtained is poured in the mould, different warm areas in 25 ℃ of-100 ℃ of following water-baths, and different accumulative total consuming time polymerization 24-72 hour obtains SiO
2The modified organic glass light-scattering material.
2,, it is characterized in that described nanometer SiO according to the method for claim 1
2The particle diameter of powder at 20nm between the 600nm.
3, according to the method for claim 1, it is characterized in that and can in step 3, add the oil soluble transparent pigment, obtain colored prepolymer after the pre-polymerization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03127636 CN1237113C (en) | 2003-07-17 | 2003-07-17 | Light scattering material of organic glass modified by Nano silicon in use for lighting and displaying, and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03127636 CN1237113C (en) | 2003-07-17 | 2003-07-17 | Light scattering material of organic glass modified by Nano silicon in use for lighting and displaying, and preparation method |
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| CN1539878A CN1539878A (en) | 2004-10-27 |
| CN1237113C true CN1237113C (en) | 2006-01-18 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8217106B2 (en) | 2005-08-03 | 2012-07-10 | Kao Corporation | Optical diffusible material |
| CN100400558C (en) * | 2005-09-09 | 2008-07-09 | 王平 | Light scattering material of heat-resistant, high strength organic glass, and prepartion method |
| CN101081919B (en) * | 2007-06-21 | 2010-06-02 | 天弘瀚（北京）科技有限公司 | Preparation method of light scattering mould plastic based on SiO2/PMMA |
| FR2918785B1 (en) * | 2007-07-13 | 2009-11-13 | Lemer Prot Anti X Par Abrevati | RADIOATTENUATOR MATERIAL, AND PROCESS FOR OBTAINING SUCH MATERIAL |
| CN103740017A (en) * | 2013-11-27 | 2014-04-23 | 南通晶鑫光学玻璃有限公司 | Modified organic glass |
| CN105037594A (en) * | 2015-05-18 | 2015-11-11 | 浙江龙游展宇有机玻璃有限公司 | Production method of flame-retarding acrylic sheet material |
| CN106543613A (en) * | 2016-11-09 | 2017-03-29 | 安徽新胜塑料科技有限公司 | A kind of low temperature resistant acryl plates |
| CN108610444A (en) * | 2018-05-24 | 2018-10-02 | 安徽新涛光电科技有限公司 | A kind of anti-aging transparent roofs organic glass |
| CN112724567B (en) * | 2020-12-21 | 2021-08-31 | 常州顺唯尔材料科技有限公司 | Heat-resistant light diffusion plate and preparation method thereof |
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