CN101220200A - Transparent organic polymer material and method for producing the same - Google Patents
Transparent organic polymer material and method for producing the same Download PDFInfo
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- CN101220200A CN101220200A CNA2007101725889A CN200710172588A CN101220200A CN 101220200 A CN101220200 A CN 101220200A CN A2007101725889 A CNA2007101725889 A CN A2007101725889A CN 200710172588 A CN200710172588 A CN 200710172588A CN 101220200 A CN101220200 A CN 101220200A
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Abstract
The invention relates to a high refractive index transparent organic polymer material of the optical material technical field and a preparation method thereof. The organic polymer material and a precursor of inorganic microparticles are put into a pressure vessel, and pressure fluid is then inlet. By infiltration of the pressure fluid to the organic polymer materials, the precursor of the inorganic microparticles is brought inside of the polymer materials by the pressure fluid. After the pressure relief reduction treatment is carried out, the high refractive index transparent organic polymer material having properties of the inorganic microparticles infiltrating and dispersing in the organic polymer materials is obtained, which contains 90 to 99.9 percent of the organic polymer materials and 0.1 to 10 percent of the inorganic nanomicropaticles. The material can be used for optical lens of glasses, magnifiers, microscopes, cameras and binoculars, etc. and other optical communication devices of photoconductive and optical fiber, etc.
Description
Technical field
The present invention relates to a kind of macromolecular material and preparation method of optical material technical field, be specifically related to a kind of high refractive index transparent organic polymer material and preparation method thereof.
Background technology
The lens materials that organic polymer materials such as plastics are made as uses such as glasses, contact lenses, Sports spectacles, lenses for optical instruments, through semicentennial development, compare with the unorganic glass eyeglass, with its unique light weight, easily process, be not easy fragmentation, transmittance and better reach advantages such as cost is low, in optical field, obtain application more and more widely, become and opticglass, optical crystal the third-largest optical material arranged side by side.Yet the organic polymer material surface hardness is low, poor heat resistance, change of refractive scope narrower (nd is between 1.35-1.7).Specific refractory power is the most important performance of optical plastics, and this has just limited the application of organic polymer material on high refractive index (nd＞1.7) optical component.Hindered application of optical plastics ground and development, the specific refractory power that therefore improves optical plastics is one of important directions of optical plastics research.The method that improves the organic polymer material specific refractory power at present mainly is divided into two kinds, and first kind is at organic polymer material surface coating or evaporation one deck high refractive index, thin film materials.This method inorganic film comes off easily, and coating is easy to generate crackle.The method of sputter coating is the price costliness also.Second kind to be inorganic nano-particle that specific refractory power is high introduce in the organic polymer material preparation organic-inorganic nanocomposite etc. by in-situ polymerization, collosol and gel or mixing method.
Find that through literature search Chinese invention patent CN 1394900 A, CN1204170C adopt high refractive index ZnS nanoparticle and polymeric matrix are prepared the high refractive index nano laminated film that can be applicable to construct fields such as optics, display device by shifting diffuse-aggregate method to prior art.The ZnS nanoparticle that at first prepares finishing forms the polymkeric substance-nanoparticle composite film material of high refractive index (the highest nd=1.85) by polymeric matrix with the repolymerization of filming after obtaining high refractive index composite material film or polymer monomer and nanoparticle colloidal sol mixing of directly filming after nanoparticle colloidal sol mixes then.This in-situ polymerization or sol-gel method complex process, the process control difficulty, and high refractive index inorganic particulate heavy addition can influence follow-up monomeric polymerization at monomer.And inorganic nano-particle is difficult to equably, is dispersed in the full-bodied polymer melt with nano level in the method for melting mixing, and not only specific refractory power is difficult to improve, and serious harm the original transparency of polymkeric substance.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of high refractive index transparent organic polymer material and preparation method thereof is provided, make it solve the problem that in polymer surfaces coating technology and collosol and gel, mixing technology, exists.The present invention utilizes the pressure fluid implantttion technique, the presoma of high refractive index inorganic fine particles is brought in the organic polymer material of eyeglass body, prepared in polymkeric substance, the composite high-molecular material that specific refractory power increases substantially, transparent of inorganic fine particles good distribution, simple, the cleaning of technology.
The present invention is achieved by the following technical solutions:
Transparent organic polymer material involved in the present invention, component that comprises and weight percent content thereof are: organic polymer material 90-99.9%, the sub-0.1%-10% of inorganic nano-particle.
The preparation method of transparent organic polymer material involved in the present invention is that organic polymer material is contacted with pressure fluid, and organic polymer material is injected inorganic fine particles simultaneously by swelling and plasticizing, makes it be dispersed in organic polymer material inside.Be specially:
The presoma of organic polymer material, inorganic fine particles is placed pressurized vessel, feed pressure fluid.The presoma of inorganic fine particles is dissolved in the pressure fluid, contact with organic polymer material by pressure fluid, pressure fluid enters organic polymer material inside, makes the organic polymer material swelling on the one hand, can be injected into macromolecular material inside to the dissolved presoma simultaneously on the one hand.Keep swelling and infiltration after 0.5～10 hour, material is taken out in release, hydrolysis at room temperature 1～2 day or at 60～140 ℃ of following pyrolysis 0.5～12h or use hydrogen reducing, make presoma be reduced into inorganic fine particles, thereby preparation have the high refractive index transparent organic polymer material that inorganic fine particles is injected, is dispersed in the feature of organic polymer material inside.
Described organic polymer material is to comprise lens materials polycarbonate (PC), polymethylmethacrylate (PMMA), allyl diglycol carbonates (CR39), and other transparent plastics Resins, epoxy for example, polyimide (PI), polystyrene (PS), ethylene glycol terephthalate (PET), transparent polyvinyl chloride (PVC), styrene-acrylonitrile copolymer (NAS), the multipolymer of vinylbenzene-methyl methacrylate (MS), transparent styrene butadiene-propylene ester (ABS), thioxanthamide (thiocarbamide alkane, thiourethane) Ju San Ring methacrylate in last of the ten Heavenly stems OZ-1000 and 1011,1012,1013 series such as grade, methacrylic acid encircles multipolymer " ARTON " resin of norbornylene ester and methyl methacrylate more, cyclic olefin polymer (COP), a kind of in the cyclic olefine copolymer (COC) etc. just is suitable for for all transparent polymer materials.
Described inorganic fine particles is a kind of in titanium oxide, zinc oxide, zinc sulphide, the zirconium white.Inorganic fine particles is dispersed in the zone that is deeper than apart from material surface 10nm.Can prevent that functional inorganic fine particles from deviating from from material surface, thereby guarantee the stable of material property.The weight content of inorganic fine particles is at 0.1%-10%.Be less than at 0.1% o'clock, nano effect can not be given full play to, and is higher than at 10% o'clock, and the specific refractory power of material can further not improve, and increases but the content height can cause eyeglass weight.Preferred content is at 0.5-5%.The diameter of inorganic fine particles is between 1-100nm, and diameter is the smaller the better.The diameter of inorganic fine particles except improving the specific refractory power of material, can also give material certain color between 10-30nm the time.
The presoma of described inorganic fine particles is alkoxide, carbonyl coordination compound, methyl ethyl diketone coordination compound, or is a kind of in the organometallic compound of main component with alkoxide, carbonyl coordination compound, methyl ethyl diketone coordination compound.For example the organometallic compound for titanium can be in tetrabutyl titanate, isopropyl titanate or metatitanic acid (four) ethyl ester a kind of.Presoma can be dissolved in the pressure fluid.
Described pressure fluid can be various, preferably to organic polymer material perviousness excellent supercutical fluid and subcritical fluids.The fluidic kind is following any: 1. carbonic acid gas: 31.1 ℃ of critical temperatures, emergent pressure 7.38MPa, 2. nitrogen protoxide: 36.4 ℃ of critical temperatures, emergent pressure 7.24MPa, 3. nitrogen: critical temperature-147 ℃, emergent pressure 3.39MPa, 4. three fluoro methane Trifluoromethane: wherein a kind of of 25.9 ℃ of critical temperatures, emergent pressure 4.83MPa.The lower limit of the temperature and pressure of operation is by the kind decision of pressure fluid.If supercritical co, then the service temperature lower limit is that 31.1 ℃ of the critical temperatures of carbonic acid gas, the lower limit of pressure are the emergent pressure 7.38MPa of carbonic acid gas such as pressure fluid.
Among the present invention, when the presoma that pressure fluid carries inorganic fine particles is injected into organic polymer material, add solubility promoter, if solubility promoter can dissolve the good solvent of presoma at least or can plastify the good solvent of organic polymer material, usually selecting lower alcohol, ketone or alkane for use, for example can be a kind of in acetone, ethanol, Virahol or the hexane.The solubility promoter addition is the 0.5%-10% of organic polymer material weight.
The high refractive index transparent macromolecular material of the present invention's preparation also has the uv-absorbing function and improves material surface scratch resistance function.
The special property that the present invention becomes inorganic fine particles by pressure fluid to the solvency action of the presoma of inorganic fine particles, swelling, osmosis and presoma facile hydrolysis to polymeric matrix or pyrolysis, the inorganic fine particles that will have high refractive index is introduced, nano-dispersed in the organic polymer material matrix, thereby a kind of novel method for preparing high refractive index and the compound organic polymer material of high transparent is provided.By the material of this method preparation, inorganic fine particles is uniformly dispersed, and material optical property homogeneous, stable has high and adjustable continuously, the transparency advantages of higher of specific refractory power.The shortcoming that can either avoid the high refractive index film in the coating method to come off, cause the organic polymer material shock resistance to reduce easily can be avoided the shortcoming in collosol and gel or the compounding process again.
The high refractive index transparent macromolecular material of the present invention's preparation can be used for various optical mirror slips, eyeglasses such as glasses lens, contact lenses, Sports spectacles, magnifying glass for example, also have lenses for optical instruments such as microscope, photographic camera, visual telescope, also can be used for the employed various transparent plastic materials of optical communication device of other photoconduction, optical fiber etc.
Description of drawings
Fig. 1 is the transmission electron microscope photo of dispersive titanium dioxide in the polycarbonate batten that obtains of embodiment 1.
Wherein: the mean diameter of titanium dioxide particle is 24nm.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The specific refractory power of raw material polycarbonate at the 589.3nm place is 1.586, and transmitance is 88.0% at the 550nm place.The polycarbonate batten of 1.8g, isopropyl titanate and the solubility promoter ethanol 0.18g of 0.4g being placed autoclave pressure jointly, feed the 99.9vol% high-pureness carbon dioxide, is 40 ℃ in temperature, and pressure is under the 15MPa, swelling and infiltration 10.0 hours; The PC batten is taken out in release; 140 ℃ of reduction 0.5 hour, obtain having the polycarbonate/titanic oxide nano compound material of high refractive index and high transparent.The weight percent content of polycarbonate is 95.77% in the material, and the weight percent content of titanium dioxide is 4.23%.Measuring the specific refractory power of material at the 589.3nm place is 2.149, and transmitance is 87.6% at the 550nm place.
The transmission electron microscope photo of dispersive titanium dioxide in the polycarbonate batten that present embodiment 1 obtains, as shown in Figure 1, the mean diameter of titanium dioxide particle is 24nm.
Embodiment 2
The specific refractory power of raw material polycarbonate at the 589.3nm place is 1.586, and transmitance is 88.0% at the 550nm place.The polycarbonate batten of 2.0g, isopropyl titanate and the solubility promoter acetone 0.1g of 0.2g being placed autoclave pressure jointly, feed the 99.9vol% high-pureness carbon dioxide, is 60 ℃ in temperature, and pressure is under the 30MPa, swelling and infiltration 6.0 hours; The PC batten is taken out in release; 110 ℃ of reduction 6.0 hours, obtain having the polycarbonate/titanic oxide nano compound material of high refractive index and high transparent.The weight percent content of polycarbonate is 98.19% in the material, and the weight percent content of titanium dioxide is 1.81%.Measuring the specific refractory power of material at the 589.3nm place is 1.963, and transmitance is 87.7% at the 550nm place.
Embodiment 3
The specific refractory power of raw material polycarbonate at the 589.3nm place is 1.586, and transmitance is 88.0% at the 550nm place.The polycarbonate batten of 2.0g, isopropyl titanate and the solubility promoter normal hexane 0.01g of 0.1g being placed autoclave pressure jointly, feed the 99.9vol% high-pureness carbon dioxide, is 80 ℃ in temperature, and pressure is under the 20MPa, swelling and infiltration 0.5 hour; The PC batten is taken out in release; 60 ℃ of reduction 12 hours, obtain having the polycarbonate/titanic oxide nano compound material of high refractive index and high transparent.The weight percent content of polycarbonate is 99.86% in the material, and the weight percent content of titanium dioxide is 0.14%.Measuring the specific refractory power of material at the 589.3nm place is 1.697, and transmitance is 87.9% at the 550nm place.
Embodiment 4
The specific refractory power of raw material polymethylmethacrylate at the 589.3nm place is 1.491, and transmitance is 92.0% at the 550nm place.The polymethylmethacrylate batten of 4.0g, tetrabutyl titanate and the solubility promoter ethanol 0.2g of 0.1g being placed autoclave pressure jointly, feed the 99.9vol% high-pureness carbon dioxide, is 40 ℃ in temperature, and pressure is under the 15MPa, swelling and infiltration 6 hours; Batten is taken out in release, 70 ℃ of reduction 6 hours, obtains having the polymethyl methacryate/titanic oxide nano composite material of high refractive index and high transparent.The weight percent content of polymethylmethacrylate is 98.68% in the material, and the weight percent content of titanium dioxide is 1.32%.Measuring the specific refractory power of material at the 589.3nm place is 1.887, and transmitance is 91.3% at the 550nm place.
Embodiment 5
The specific refractory power of raw material polystyrene at the 589.3nm place is 1.590, and transmitance is 90.0% at the 550nm place.The polystyrene batten of 2.0g, titanium ethanolate and the solubility promoter ethanol 0.1g of 0.1g being placed autoclave pressure jointly, feed the 99.9vol% high-pureness carbon dioxide, is 40 ℃ in temperature, and pressure is under the 15MPa, swelling and infiltration 6 hours; Batten is taken out in release, 70 ℃ of reduction 4 hours, obtains having the polystyrene/titanic oxide nano compound material of high refractive index and high transparent.The weight percent content of polystyrene is 98.23% in the material, and the weight percent content of titanium dioxide is 1.77%.Measuring the specific refractory power of material at the 589.3nm place is 2.014, and transmitance is 89.4% at the 550nm place.
Embodiment 6
The specific refractory power of raw material allyl diglycol carbonates (CR39) at the 589.3nm place is 1.498, and transmitance is 92.0% at the 550nm place.The CR39 batten of 2.0g, tetrabutyl titanate and the solubility promoter ethanol 0.1g of 0.1g being placed autoclave pressure jointly, feed the 99.9vol% high-pureness carbon dioxide, is 40 ℃ in temperature, and pressure is under the 20MPa, swelling and infiltration 6 hours; Batten is taken out in release, 60 ℃ of reduction 10 hours, obtains having the CR39/ titanic oxide nano compound material of high refractive index and high transparent.The weight percent content of CR39 is 97.36% in the material, and the weight percent content of titanium dioxide is 2.64%.Measuring the specific refractory power of material at the 589.3nm place is 1.834, and transmitance is 90.7% at the 550nm place.
Claims (10)
1. transparent organic polymer material, it is characterized in that, component that comprises and weight percent content thereof are: organic polymer material 90-99.9%, the sub-0.1%-10% of inorganic nano-particle, described organic polymer material is a kind of in all transparent polymer materials, described inorganic fine particles is a kind of in titanium oxide, zinc oxide, zinc sulphide, the zirconium white, and inorganic nano-particle injects, is dispersed in swollen organic polymer material inside.
2. transparent organic polymer material according to claim 1 is characterized in that: described inorganic fine particles is injected, is dispersed in the zone that is deeper than apart from organic polymer material surface 10nm, and the diameter of inorganic fine particles is 1nm-100nm.
3. transparent organic polymer material according to claim 1 and 2 is characterized in that: the weight percent content of described inorganic fine particles is 0.5%-5%, and the inorganic fine particles diameter is 10nm-30nm.
4. transparent organic polymer material according to claim 1 and 2, it is characterized in that: described organic polymer material is to comprise polycarbonate, polymethylmethacrylate, allyl diglycol carbonates, Resins, epoxy, polyimide, polystyrene, ethylene glycol terephthalate, transparent polyvinyl chloride, styrene-acrylonitrile copolymer, the multipolymer of vinylbenzene-methyl methacrylate, transparent styrene butadiene-propylene ester, thioxanthamide Ju San Ring methacrylate in the last of the ten Heavenly stems, methacrylic acid encircles the copolymer A RTON resin of norbornylene ester and methyl methacrylate more, cyclic olefin polymer, a kind of in the cyclic olefine copolymer.
5. the preparation method of a transparent organic polymer material as claimed in claim 1, it is characterized in that: with organic polymer material, the presoma of inorganic fine particles places pressurized vessel, feed pressure fluid, the presoma of inorganic fine particles is dissolved in the pressure fluid, contact with organic polymer material by pressure fluid, pressure fluid enters organic polymer material inside, make the organic polymer material swelling, simultaneously the dissolved presoma is injected into macromolecular material inside, after keeping swelling and permeating for some time, take out material, hydrolysis or pyrolysis or use hydrogen reducing, make presoma be reduced into inorganic fine particles, inject thereby obtain having inorganic fine particles, be dispersed in the high refractive index transparent organic polymer material of organic polymer material inside.
6. the preparation method of transparent organic polymer material as claimed in claim 5, it is characterized in that: when the presoma that described pressure fluid carries inorganic fine particles is injected into organic polymer material, add solubility promoter, the solubility promoter addition is the 0.5%-10% of organic polymer material weight.
7. the preparation method of transparent organic polymer material as claimed in claim 6, it is characterized in that: described solubility promoter is a kind of in acetone, ethanol, Virahol or the hexane.
8. the preparation method of transparent organic polymer material as claimed in claim 5, it is characterized in that: the presoma of described inorganic fine particles is alkoxide, carbonyl coordination compound, methyl ethyl diketone coordination compound, or be a kind of in the organometallic compound of main component with alkoxide, carbonyl coordination compound, methyl ethyl diketone coordination compound, this presoma can be dissolved in the pressure fluid.
9. as the preparation method of claim 5 or 8 described transparent organic polymer materials, it is characterized in that: described pressure fluid is supercutical fluid and subcritical fluids, is in following any:
Carbonic acid gas: 31.1 ℃ of critical temperatures, emergent pressure 7.38MPa;
Nitrogen protoxide: 36.4 ℃ of critical temperatures, emergent pressure 7.24MPa;
Nitrogen: critical temperature-147 ℃, emergent pressure 3.39MPa;
Three fluoro methane: 25.9 ℃ of critical temperatures, emergent pressure 4.83MPa.
10. the preparation method of transparent organic polymer material as claimed in claim 5 is characterized in that: described maintenance swelling and infiltration for some time, be meant to keep swelling and infiltration 0.5h～10h; Described hydrolysis was meant hydrolysis at room temperature 1 day～2 days; Described pyrolysis is meant at 60 ℃～140 ℃ following pyrolysis 0.5h～12h.
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| CN102445716A (en) * | 2010-10-12 | 2012-05-09 | 鸿富锦精密工业（深圳）有限公司 | Lens and manufacturing method as well as manufacturing equipment of lens |
| CN103396566A (en) * | 2013-07-18 | 2013-11-20 | 上海交通大学 | Preparation method of polymethyl methacrylate/zirconium dioxide composite material |
| CN104031525A (en) * | 2014-06-04 | 2014-09-10 | 绍兴京华激光制品有限公司 | Coating liquid with high refractive index for transparent holographic film and preparation method thereof |
| CN104086933A (en) * | 2014-07-29 | 2014-10-08 | 上海海昌医用塑胶厂 | COC bottle and preparation method thereof |
| CN104672717A (en) * | 2015-03-06 | 2015-06-03 | 苏州市景荣科技有限公司 | Preparation method of nano titanium oxide modified PVC (polyvinyl chloride) resin |
| RU2561278C1 (en) * | 2014-07-07 | 2015-08-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный университет" | Method of obtaining transparent metal-containing polymerisable compositions |
| CN106366533A (en) * | 2016-08-30 | 2017-02-01 | 东兴华鸿光学科技有限公司 | Optical lens with low thermal conductivity |
| CN106589754A (en) * | 2016-12-20 | 2017-04-26 | 安徽亚克力实业有限公司 | Impact-resistant organic glass and preparation method thereof |
| CN108148390A (en) * | 2017-12-23 | 2018-06-12 | 洛阳名力科技开发有限公司 | Resin eyeglass |
| CN110450250A (en) * | 2019-06-26 | 2019-11-15 | 华南农业大学 | A kind of hydrophobic film structure and preparation method thereof, mould-proof-type timber |
| CN113831709A (en) * | 2021-09-13 | 2021-12-24 | 淄博中南医药包装材料股份有限公司 | Biodegradable magnifier |
| WO2022126647A1 (en) * | 2020-12-18 | 2022-06-23 | 清华大学 | High-temperature energy storage hybrid polyetherimide dielectric thin film, preparation method therefor and use thereof |
| US11680163B2 (en) | 2017-10-13 | 2023-06-20 | Panasonic Intellectual Property Management Co., Ltd. | Resin composition for optical waveguide cores, and dry film, optical waveguide core and photoelectric composite wiring board, each of which uses same |
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- 2007-12-20 CN CNA2007101725889A patent/CN101220200A/en active Pending
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| CN102445716A (en) * | 2010-10-12 | 2012-05-09 | 鸿富锦精密工业（深圳）有限公司 | Lens and manufacturing method as well as manufacturing equipment of lens |
| CN103396566A (en) * | 2013-07-18 | 2013-11-20 | 上海交通大学 | Preparation method of polymethyl methacrylate/zirconium dioxide composite material |
| CN103396566B (en) * | 2013-07-18 | 2015-12-09 | 上海交通大学 | The preparation method of polymethyl methacrylate/zirconidioxide dioxide composite material |
| CN104031525A (en) * | 2014-06-04 | 2014-09-10 | 绍兴京华激光制品有限公司 | Coating liquid with high refractive index for transparent holographic film and preparation method thereof |
| RU2561278C1 (en) * | 2014-07-07 | 2015-08-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный университет" | Method of obtaining transparent metal-containing polymerisable compositions |
| CN104086933A (en) * | 2014-07-29 | 2014-10-08 | 上海海昌医用塑胶厂 | COC bottle and preparation method thereof |
| CN104672717A (en) * | 2015-03-06 | 2015-06-03 | 苏州市景荣科技有限公司 | Preparation method of nano titanium oxide modified PVC (polyvinyl chloride) resin |
| CN106366533A (en) * | 2016-08-30 | 2017-02-01 | 东兴华鸿光学科技有限公司 | Optical lens with low thermal conductivity |
| CN106589754A (en) * | 2016-12-20 | 2017-04-26 | 安徽亚克力实业有限公司 | Impact-resistant organic glass and preparation method thereof |
| US11680163B2 (en) | 2017-10-13 | 2023-06-20 | Panasonic Intellectual Property Management Co., Ltd. | Resin composition for optical waveguide cores, and dry film, optical waveguide core and photoelectric composite wiring board, each of which uses same |
| CN108148390A (en) * | 2017-12-23 | 2018-06-12 | 洛阳名力科技开发有限公司 | Resin eyeglass |
| CN110450250A (en) * | 2019-06-26 | 2019-11-15 | 华南农业大学 | A kind of hydrophobic film structure and preparation method thereof, mould-proof-type timber |
| WO2022126647A1 (en) * | 2020-12-18 | 2022-06-23 | 清华大学 | High-temperature energy storage hybrid polyetherimide dielectric thin film, preparation method therefor and use thereof |
| CN113831709A (en) * | 2021-09-13 | 2021-12-24 | 淄博中南医药包装材料股份有限公司 | Biodegradable magnifier |
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