CN111116990B - Ultraviolet-blue light absorbent, preparation method thereof and prepared ultraviolet-blue light absorbent material - Google Patents
Ultraviolet-blue light absorbent, preparation method thereof and prepared ultraviolet-blue light absorbent material Download PDFInfo
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- CN111116990B CN111116990B CN201911114182.4A CN201911114182A CN111116990B CN 111116990 B CN111116990 B CN 111116990B CN 201911114182 A CN201911114182 A CN 201911114182A CN 111116990 B CN111116990 B CN 111116990B
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Abstract
The invention belongs to the field of materials, and discloses an ultraviolet-blue light absorbent, a preparation method thereof and a prepared ultraviolet-blue light absorbent material. The ultraviolet-blue light absorber has a structure shown as the following formula (I), wherein R is-OH or-NH2. And preparing the ultraviolet-blue light absorbing material by using the ultraviolet-blue light absorber, the methyl methacrylate, the polymethyl methacrylate and the initiator together. The optical property of carbon dots in the ultraviolet-blue light absorber is utilized to well absorb high-energy ultraviolet-blue light in an external light source. The obtained ultraviolet-blue light absorbing material has good permeability and can absorb harmful ultraviolet light and blue light. The preparation method provided by the invention is simple to operate, has low requirements on equipment and low cost, and the product can be applied to instrument panels, lamp tubes, decorative glass, mobile phone screen protective films, spectacle lenses and the like.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to an ultraviolet-blue light absorbent, a preparation method thereof and a prepared ultraviolet-blue light absorbent material.
Background
Among visible light, ultraviolet light is the most energetic light, and irradiation of ultraviolet light in a large amount causes premature aging of the skin and even induces skin cancer, while short wavelength light of high energy has blue light in addition to ultraviolet light. Blue light has higher energy, and the damage to the human body is mainly damage to the retina of the eye, which can cause myopia and even blindness. However, except sunlight, blue light can be seen everywhere in daily life, and blue light exists in mobile phones, computers, LED display screens and fluorescent lamps, so that new problems cannot be caused by technological progress, and people can enjoy the hidden injuries conveniently and quickly. The electronic products emit a large amount of short-wave blue light, and the blue light can penetrate through crystalline lens to directly reach retina, so that fundus pathological injuries such as myopia, maculopathy and the like are caused, and the secretion of melatonin is inhibited, so that insomnia is caused. The wavelength of blue light is between 400-500nm, and the most harmful is between 400-450 nm.
Polymethyl methacrylate (PMMA) can effectively filter ultraviolet light with the wavelength less than 300nm, but the filtering effect between 300nm and 400nm is poor. The light after 400nm is even less filtered out, so that the incorporation of carbon dots into PMMA both transmits and absorbs harmful light.
Disclosure of Invention
To overcome the disadvantages and shortcomings of the prior art, it is a primary object of the present invention to provide an ultraviolet-blue light absorber.
It is still another object of the present invention to provide a method for preparing the above ultraviolet-blue light absorber.
It is still another object of the present invention to provide an ultraviolet-blue light absorbing material made of the above ultraviolet-blue light absorber; the material has an absorption wavelength of 300-475nm, and can effectively absorb high-energy ultraviolet light and blue light by using the optical characteristics of carbon dots as an absorbent.
The invention also aims to provide a preparation method of the ultraviolet-blue light absorbing material.
Still another object of the present invention is to provide a use of the above ultraviolet-blue light absorbing material; can be applied to lamp tubes, indication boards, instrument dials, decorative doors and windows, mobile phone screen protective films, spectacle lenses and the like in life.
The purpose of the invention is realized by the following technical scheme:
an ultraviolet-blue light absorber having the structure of formula (i):
wherein R is-OH or-NH2。
The preparation method of the ultraviolet-blue light absorber comprises the following operation steps:
(1) weighing Ethylene Diamine Tetraacetic Acid (EDTA) and ethanolamine with a molar ratio of 1:3, and adding water to dissolve to obtain a mixture;
(2) carrying out oil bath reflux reaction on the mixture, then centrifuging, removing insoluble precipitate, and keeping supernatant;
(3) and carrying out suction filtration on the supernatant liquid, and removing large-particle-size molecules in the solution to obtain the ultraviolet-blue light absorbent.
The oil bath reflux reaction in the step (2) is carried out for 8-12h at the temperature of 200 ℃; the centrifugation times are 3-4, the rotation speed of each centrifugation is 5000-10000rpm, and the centrifugation time is 5-10 minutes.
And (3) performing suction filtration by adopting a sand core funnel and an aqueous phase filter membrane with the aperture of 0.22 mu m.
An ultraviolet-blue light absorbing material prepared from the ultraviolet-blue light absorbent is prepared from the following raw materials in parts by weight: 20-30 parts of methyl methacrylate, 0.5-1 part of polymethyl methacrylate, 0.2-0.4 part of initiator and 1-4 parts of ultraviolet-blue light absorbent.
The initiator is tert-butyl peroxybenzoate or dicumyl peroxide.
The preparation method of the ultraviolet-blue light absorbing material comprises the following operation steps:
(1) weighing and mixing methyl methacrylate and polymethyl methacrylate, stirring, heating in a water bath to 80-90 ℃, continuously heating for 1h after reactants are dissolved, stopping heating, and cooling to 50 ℃ by using a cold water bath;
(2) adding ultraviolet-blue light absorbent and continuing stirring, adding initiator, uniformly stirring, taking out, putting into an oven with the temperature of 40-50 ℃ for 6-8 days to enable the mixture to reach a solidification state, further heating to the temperature of 100 ℃ and 110 ℃ for high-temperature heat treatment to enable the mixture to be fully polymerized, and finally obtaining the ultraviolet-blue light absorbent material product.
The ultraviolet-blue light absorbing material is applied to instrument panels, lamp tubes, decorative glass, mobile phone screen protective films and spectacle lenses.
The ultraviolet-blue light absorber of the present invention is composed of carbon dots. When high-energy light irradiates the carbon point, valence electrons in the carbon point transition to a higher energy level and occupy an inverted bond orbit, so that the absorption wavelength is in the ultraviolet-blue light region, namely 300-475 nm. The ultraviolet-blue light absorbent is further utilized to prepare the ultraviolet-blue light absorbent material, and the carbon dots contain ester groups, carboxyl groups, amino groups and the like, and can form hydrogen bonds with methyl methacrylate and an initiator so as to be fixed and uniformly dispersed in the ultraviolet-blue light absorbent material, so that the carbon dots can absorb corresponding ultraviolet-blue light while ensuring the light transmission in the polymethyl methacrylate, and the performance of the ultraviolet-blue light absorbent material is not influenced. The ultraviolet-blue light absorbing material can effectively absorb ultraviolet light and blue light in an external light source, thereby playing a role in protecting vision, and can be applied to instrument panels, lamp tubes, decorative glass, mobile phone screen protective films, glasses lenses and the like.
Compared with the prior art, the invention has the following advantages and effects:
(1) the ultraviolet-blue light absorbing material product prepared by the invention has good functions of absorbing ultraviolet light (300-; the carbon dots are simple to synthesize, low in cost, environment-friendly, stable in optical property and rich in organic groups on the surface, can be well dispersed in the polymethyl methacrylate, reduces the using amount of an initiator in the polymerization reaction process of the methyl methacrylate, and can absorb ultraviolet-blue light in a certain range so as to reduce the damage of lamplight or sunlight to a human body; meanwhile, the polymethyl methacrylate has good light transmittance, the ultraviolet-blue light absorbing material can ensure the permeation of other light while removing harmful light, and normal light utilization is not influenced, thus being easy to manufacture and use.
(2) The carbon dots contain ester groups, carboxyl groups, amino groups and the like, and can form hydrogen bonds with the methyl methacrylate and the initiator so as to be fixed and uniformly dispersed in the carbon dots, so that the carbon dots can absorb corresponding ultraviolet-blue light while ensuring the light transmission in the polymethyl methacrylate, and the performance of the carbon dots is not influenced.
Drawings
FIG. 1 is a Fourier transform infrared spectrum of the UV-blue absorber (carbon dots) prepared in example 1.
FIG. 2 is a transmission electron micrograph and a high resolution transmission electron micrograph of the UV-blue absorber (carbon dots) prepared in example 1; the particle size of the carbon dots is less than 10nm, the carbon dots are irregular spheres, and the top right-hand insert is a high-resolution transmission electron microscope image, which shows that the interplanar spacing of the carbon dots is 0.21nm, which is 100 planes of graphite, and shows that the carbon dots have good crystallization performance and high graphitization degree.
FIG. 3 is a UV-visible absorption spectrum of carbon dots (i.e., UV-blue light absorber), neat PMMA, and a UV-blue light absorbing material prepared from carbon dots and PMMA prepared in example 1; pure PMMA can only absorb ultraviolet light with the wavelength of 300-375nm, and the ultraviolet-blue light absorbing material made of the carbon dots and PMMA can absorb ultraviolet light and blue light with the wavelength range of 300-500 nm.
Detailed description of the invention
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
an ultraviolet-blue light absorber is prepared according to the following preparation method:
(1) adding 5.14mmol of EDTA, 15.42mmol of ethanolamine and 50mL of deionized water into a 250mL three-neck flask, fully dissolving, and carrying out oil bath reflux reaction at 200 ℃ for 10h to obtain a mixture;
(2) centrifuging the mixture 3 times at 8000rpm for 8 min, removing precipitate, and retaining supernatant;
(3) and carrying out suction filtration on the obtained supernatant by using a sand core funnel, using an aqueous phase filter membrane with the aperture of 0.22 mu m, and removing large-particle-size molecules in the solution to finally obtain the ultraviolet-blue light absorbent. FIG. 1 is a Fourier transform infrared spectrum of the ultraviolet absorbent, and it can be seen from FIG. 1 that the prepared ultraviolet-blue absorbent is a carbon dot surface containing abundant organic groups, such as amino, carboxyl and hydroxyl. As shown in fig. 2, the transmission electron micrograph of the carbon dots shows that the ultraviolet-blue light absorber has a particle size of less than 10nm and is in an irregular spherical shape. The insert in the upper right corner is a high-resolution transmission electron microscope image of the carbon dots, and shows that the interplanar spacing of the carbon dots is 0.21nm, which is 100 planes of graphite, and shows that the carbon dots have good crystallization performance and higher graphitization degree. From the above structural characterization results and analysis of the uv-blue light absorber, it can be determined that the uv-blue light absorber (carbon dots) has the following structure:
wherein R is-OH or-NH2。
The ultraviolet-blue light absorbing material prepared by using the obtained ultraviolet-blue light absorber and PMMA is prepared by the following specific preparation method:
(1) weighing 20 parts by mass of methyl methacrylate and 0.5 part by mass of polymethyl methacrylate (PMMA) in a 250mL three-neck flask, violently stirring and heating in a water bath for 80 ℃, continuously heating for 1h after reactants are dissolved, and then stopping heating and reducing the temperature to 50 ℃ by using a cold water bath.
(2) Adding 1 part by mass of ultraviolet-blue light absorber, continuously stirring, adding 0.2 part by mass of tert-butyl peroxybenzoate, uniformly stirring, taking out, putting into a 40 ℃ oven for 7 days to enable the mixture to reach a basic solidification state, further heating to 100 ℃ to carry out high-temperature heat treatment, fully polymerizing the mixture, and finally obtaining the product.
The uv-vis absorption spectra of the carbon dots (i.e., uv-blue absorber), neat PMMA, and uv-blue absorbing material prepared from the carbon dots and PMMA of example 1 are shown in fig. 3: pure PMMA can only absorb ultraviolet light with the wavelength of 300-375nm, and the ultraviolet-blue light absorbing material made of the carbon dots and PMMA can absorb ultraviolet light and blue light with the wavelength range of 300-500 nm.
Example 2:
an ultraviolet-blue light absorber was synthesized with reference to example 1. The obtained ultraviolet-blue light absorbent is used for preparing an ultraviolet-blue light absorbing material, and the preparation method specifically comprises the following steps:
(1) weighing 25 parts by mass of methyl methacrylate and 1 part by mass of polymethyl methacrylate in a 250mL three-neck flask, violently stirring and heating in a water bath for 90 ℃, continuously heating for 1h after reactants are dissolved, then stopping heating and cooling to 50 ℃ by using a cold water bath.
(2) Adding 3 parts by mass of ultraviolet-blue light absorbent, continuously stirring, adding 0.2 part by mass of dicumyl peroxide, uniformly stirring, taking out, putting into a 50 ℃ oven for 7 days to enable the mixture to reach a basic solidification state, further heating to 110 ℃ to carry out high-temperature heat treatment, fully polymerizing the mixture, and finally obtaining the product.
Example 3:
an ultraviolet-blue light absorber was synthesized with reference to example 1. The obtained ultraviolet-blue light absorbent is used for preparing an ultraviolet-blue light absorbing material, and the preparation method specifically comprises the following steps:
(1) weighing 30 parts by mass of methyl methacrylate and 1 part by mass of polymethyl methacrylate in a 250mL three-neck flask, violently stirring and heating in a water bath at 85 ℃, continuously heating for 1h after reactants are dissolved, then stopping heating and cooling to 50 ℃ by using a cold water bath.
(2) Adding 4 parts by mass of ultraviolet-blue light absorbent, continuously stirring, adding 0.4 part by mass of dicumyl peroxide, uniformly stirring, taking out, putting into a 45 ℃ oven for 7 days to enable the mixture to reach a basic solidification state, further heating to 105 ℃ for high-temperature heat treatment, fully polymerizing, and finally obtaining the product.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of an ultraviolet-blue light absorber is characterized by comprising the following operation steps:
(1) weighing ethylene diamine tetraacetic acid and ethanolamine with a molar ratio of 1:3, and adding water for dissolving to obtain a mixture;
(2) carrying out oil bath reflux reaction on the mixture at 200 ℃ for 10h, then centrifuging for 3 times, wherein the rotating speed of each centrifugation is 8000rpm, the centrifuging time is 8 minutes, removing insoluble precipitate, and keeping supernatant;
(3) and (3) carrying out suction filtration on the supernatant by adopting a sand core funnel and an aqueous phase filter membrane with the aperture of 0.22 mu m, and removing large-particle-size molecules in the solution to obtain the ultraviolet-blue light absorbent.
2. An ultraviolet-blue light absorber prepared by the preparation method of claim 1.
3. An ultraviolet-blue light absorbing material made from the ultraviolet-blue light absorber of claim 2, wherein: the material is prepared from the following raw materials in parts by weight: 20-30 parts of methyl methacrylate, 0.5-1 part of polymethyl methacrylate, 0.2-0.4 part of initiator and 1-4 parts of ultraviolet-blue light absorbent.
4. The uv-blue absorbing material of claim 3, wherein: the initiator is tert-butyl peroxybenzoate or dicumyl peroxide.
5. A method for preparing a uv-blue absorbing material according to claim 3, characterized in that it comprises the following operative steps:
(1) weighing and mixing methyl methacrylate and polymethyl methacrylate, stirring, heating in a water bath to 80-90 ℃, continuously heating for 1h after reactants are dissolved, stopping heating, and cooling to 50 ℃ by using a cold water bath;
(2) adding ultraviolet-blue light absorbent and continuing stirring, adding initiator, uniformly stirring, taking out, putting into an oven with the temperature of 40-50 ℃ for 6-8 days to enable the mixture to reach a solidification state, further heating to the temperature of 100 ℃ and 110 ℃ for high-temperature heat treatment to enable the mixture to be fully polymerized, and finally obtaining the ultraviolet-blue light absorbent material product.
6. Use of the uv-blue absorbing material according to claim 3 in dashboards, light tubes, decorative glass, protective films for cell phone screens, spectacle lenses.
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| CN113652224B (en) * | 2021-01-31 | 2024-02-23 | 重庆大学 | Anti-quenching carbon quantum dot solid compound, blue light prevention film and preparation method thereof |
| CN113603834A (en) * | 2021-08-05 | 2021-11-05 | 深圳市辉灿科技有限公司 | Preparation method of liquid for absorbing blue light of LED light source and low-blue-light LED lamp |
| CN113671615B (en) * | 2021-08-20 | 2023-08-25 | 辽宁石化职业技术学院 | High-frequency blue light shielding method |
| CN117757470A (en) * | 2023-12-07 | 2024-03-26 | 扬州大学 | Grass carbon dot and preparation method and application thereof |
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