CN114983849B - Single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel and preparation and application thereof - Google Patents
Single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel and preparation and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of tooth whitening, and relates to single-component low-hydrogen-peroxide-concentration visible light-catalyzed tooth whitening gel, and preparation and application thereof. The tooth whitening gel consists of copper-iron co-doped nano titanium dioxide, a light stabilizer, a gel agent, hydrogen peroxide, a desensitizer, a whitening filler, an auxiliary agent and deionized water. The nanometer titanium dioxide in the tooth whitening gel is prepared by a hydrothermal method, has visible light catalytic activity, and can be used for synergistic catalytic decomposition of hydrogen peroxide. The mass concentration of hydrogen peroxide in the whitening gel is less than 3%, the storage time at room temperature is more than 12 months, and the whitening effect on teeth can be remarkably improved after 10 times of use.
Description
Technical Field
The invention belongs to the technical field of tooth whitening, and relates to single-component low-hydrogen-peroxide-concentration visible light-catalyzed tooth whitening gel, and preparation and application thereof.
Background
Nano titanium dioxide is a novel inorganic nano material developed by the end of the 80 th century. The ultraviolet light-absorbing material has the advantages of large specific surface area, strong ultraviolet light absorbing capability, good thermal conductivity, large surface activity, good dispersibility and wide attention. However, the larger forbidden bandwidth of the nano titanium dioxide determines that the nano titanium dioxide can only be excited by ultraviolet light with higher energy, so that visible light catalysis can not be realized, and the application of the nano titanium dioxide in the field of visible light catalysis tooth whitening gel is limited. In the tooth whitening gel, the visible light catalytic whitening gel is generally adopted to realize the tooth whitening function, so that the application of the nano titanium dioxide in the whitening gel is limited. The metal ion doping method is to dope metal ions into titanium dioxide crystal lattices to form impurity energy levels and reduce forbidden band width, so that the photoresponse range of the titanium dioxide is widened, and the effect of visible light catalysis is realized. The whitening gel is a tooth whitening technology popular in Europe and America, and although the whitening gel technology is mature, the existing visible light irradiation tooth whitening gel products on the market still have some problems. Firstly, the concentration of hydrogen peroxide in the gel is higher, the concentration of the hydrogen peroxide is generally more than 5%, partial products even reach 10%, the high-concentration hydrogen peroxide has better whitening effect, but the gingiva and the oral cavity are damaged at the same time, and the tooth pain is obvious after the gel is used; secondly, the utilization rate of the visible light whitening gel to hydrogen peroxide is low, the catalytic oxidation performance of the visible light irradiation to the hydrogen peroxide is limited, and the whitening gel can not achieve the tooth whitening effect in a short time. Meanwhile, the storage stability of the existing whitening gel is poor, and the whitening gel can be obviously thinned during storage and transportation.
Therefore, how to develop a tooth whitening gel which can be catalyzed and oxidized by mild light, such as visible light, and can generate OH by being cooperated with hydrogen peroxide decomposition, and simultaneously prolong the storage time of the whitening gel is a problem to be solved for improving the safety and reliability of the tooth whitening technology.
Disclosure of Invention
The invention mainly aims to provide a single-component low-hydrogen-peroxide-concentration visible light-catalyzed tooth whitening gel, and preparation and application thereof.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel comprises the following components in parts by weight: 10 to 15 parts of copper-iron co-doped nano titanium dioxide, 0.01 to 0.1 part of light stabilizer, 2 to 3 parts of gel, 3 to 9 parts of 30 percent hydrogen peroxide, 0.1 to 2 parts of desensitizer, 0.1 to 0.5 part of auxiliary agent, 0.5 to 1.0 part of whitening filler and 10 to 82 parts of deionized water.
The copper-iron co-doped nano titanium dioxide is prepared into porous spherical copper-iron co-doped nano titanium dioxide by a hydrothermal method.
The method comprises the steps of dissolving butyl titanate in butanol solution, marking as solution A, adding ferric nitrate and copper nitrate solution into concentrated hydrochloric acid solution, marking as solution B, dropwise adding the solution B into the solution A under low-speed stirring to form a mixed solution, carrying out hydrothermal reaction on the mixed solution in a reaction kettle at 150-300 ℃ for 8-12 hours, carrying out centrifugal separation, washing with ethanol and deionized water in sequence, and calcining for 3-4 hours at 500-650 ℃ in a muffle furnace to obtain the copper-iron co-doped titanium dioxide nano powder.
The copper-iron co-doped nano titanium dioxide is prepared by dissolving butyl titanate in butanol solution, marking as solution A, adding ferric nitrate and copper nitrate solution into concentrated hydrochloric acid solution, marking as solution B, dropwise adding the solution B into the solution A under low-speed stirring to form a mixed solution, carrying out hydrothermal reaction on the mixed solution in a reaction kettle at 150-300 ℃ for 8-12 hours, centrifuging, washing, and calcining in a muffle furnace at 500-650 ℃ for 3-4 hours to obtain the copper-iron co-doped nano titanium dioxide powder.
The whitening filler is obtained by carrying out surface chemical grafting modification on filler substances through organic resin; wherein the filler material is one or more of nano zinc oxide, quartz powder and/or titanium dioxide.
The surface chemical grafting modification is to adopt organic resin to carry out chemical grafting modification on the surface of a filler substance in an organic solvent; wherein the organic resin is one or more of epoxy resin, acrylic resin and polyester resin; the organic solvent is one or more of xylene, n-butanol and ethyl acetate.
The mass ratio of the organic resin to the filler substance is 1: 20-1: 50.
the stabilizer comprises the following components in percentage by mass: 1 to 1:5 and a light absorber, wherein the antioxidant is 2, 6-tertiary butyl-4-methylphenol and/or bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide, and the light absorber is dihydroartemisinin, erythromycin and kanamycin.
The gel is carbomer and/or carboxymethyl cellulose; the desensitizer is calcium fluoride, sodium monofluorophosphate, strontium fluoride or strontium acetate; the auxiliary agent is disodium ethylenediamine tetraacetate, glycerol or polyethylene glycol.
A preparation method of single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel comprises the following steps:
1) Adding the gel into deionized water for soaking, adding an auxiliary agent, and performing ultrasonic dispersion to obtain a mixture A;
2) Adding a stabilizer into the mixture A, uniformly stirring, adding copper-iron co-doped titanium dioxide, and uniformly stirring to obtain a mixture B;
3) Uniformly dispersing filler substances into an organic solvent, adding organic resin to perform chemical grafting modification on the filler substances, performing centrifugal separation, and cleaning with deionized water to obtain a whitening filler C;
4) Mixing the mixture B with the whitening filler C, adding 30% hydrogen peroxide by mass fraction, uniformly mixing, adding a desensitizing agent and a stabilizing agent, and regulating the pH value by using an alkali solution to obtain a mixture D, thus obtaining the tooth whitening gel.
In the step 1), the soaking time of the gel is 12-24 hours, and the soaking temperature is 5-35 ℃;
in the step 2), the stirring time is 2-4 hours, and the rotating speed is 200-400 r/min;
in the step 3), the chemical grafting modification time of the organic resin to the filler is 6-12 hours;
in the step 4), the pH value of the gel is regulated to be in the range of pH 6.5-7.5 by the alkali solution.
The application of a single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel in tooth whitening under photocatalysis.
The visible light wavelength of the photocatalyst is 400-800 nm, and the irradiation time is 30-60 min.
The application process is that the tooth whitening gel is smeared on teeth, the teeth are irradiated by LED visible light for a certain time, the visible light catalyzes nano titanium dioxide to generate oxidation electron holes, hydrogen peroxide to generate hydroxyl free radicals (OH) with strong oxidability and whitening filler, and the three cooperate to complete the tooth whitening effect.
Compared with the prior art, the invention has the following technical progress:
the active component copper-iron co-doped titanium dioxide of the tooth whitening gel has visible light excitation activity, forms electron holes with strong oxidizing property under the irradiation of visible light, and can also synergistically catalyze and decompose hydrogen peroxide to generate OH, and the electron holes and OH can both rapidly oxidize pigment and dirt on the surface of the tooth, so that the whitening effect of the tooth whitening gel on the tooth is improved;
according to the tooth whitening gel disclosed by the invention, the organic resin chemical medium modified whitening filler is added, so that the whitening effect of the gel on teeth can be improved by the whitening filler, and meanwhile, the storage stability of the whitening gel is not reduced.
The tooth whitening gel disclosed by the invention is a single-component gel, the concentration of hydrogen peroxide is less than 3%, the harm to gums is small, the safety and the high efficiency are realized, the operation is convenient, and the gel is suitable for industrial production.
Drawings
FIG. 1 is a graph of the ultraviolet diffuse reflection spectrum of the copper-iron co-doped titanium dioxide nano powder prepared in example 1 according to the embodiment of the invention.
Fig. 2 is an XRD spectrum of the copper-iron co-doped titanium dioxide nano powder prepared in example 1 provided in the example of the present invention.
Fig. 3 is an electronic scanning electron microscope photograph of the copper-iron co-doped titanium dioxide nano powder prepared in the embodiment 2 provided by the embodiment of the invention, wherein the left image is magnified 1000 times, and the right image is magnified 3000 times.
Fig. 4 is an electronic scanning electron microscope photograph of the coated nano zinc oxide prepared in example 1 provided in the embodiment of the present invention, the left image is magnified 2000 times, and the right image is magnified 3000 times.
Detailed Description
The invention will now be described in further detail by way of specific examples, which are to be understood as illustrative only and not limiting.
The nano titanium dioxide in the tooth whitening gel is prepared into a porous sphere by a hydrothermal method, has visible light catalytic activity, and can be used for synergistic catalytic decomposition of hydrogen peroxide. The mass concentration of hydrogen peroxide in the whitening gel is less than 3%, the storage time at room temperature is more than 12 months, and the whitening effect on teeth can be remarkably improved after 10 times of use.
Example 1A visible light tooth whitening gel, method of making and use
1) Preparation of copper-iron co-doped titanium dioxide and coated whitening filler
15mL of butyl titanate is dissolved in 50mL of n-butyl alcohol solution and is marked as solution A, another 3mL of 0.5M ferric nitrate and 0.3mL of 0.1M copper nitrate solution are added into 10mL of concentrated hydrochloric acid solution and are marked as solution B, the solution B is slowly dripped into the solution A under the magnetic stirring of 200 r/mm to form a mixed solution, the mixed solution is subjected to hydrothermal reaction for 10 hours in a sealed reaction kettle at 200 ℃, supernatant is removed by centrifugal separation, ethanol and deionized water are sequentially used for washing for 5 times respectively, and the mixed solution is calcined in a muffle furnace at 630 ℃ for 4 hours to obtain copper-iron co-doped titanium dioxide nano powder (see figure 1).
FIG. 1 is an ultraviolet diffuse reflection spectrum of copper-iron co-doped titanium dioxide nano powder, and the ultraviolet diffuse reflection spectrum shows that the copper-iron co-doped titanium dioxide has more excellent visible light catalytic performance. Fig. 2 is an XRD spectrum of the preparation of copper-iron co-doped titanium dioxide nano-powder, where copper and iron elements have been doped into the titanium dioxide crystal structure.
Dispersing 0.8Kg nano zinc oxide into 200mL of xylene solution at high speed, adding 40g of thermoplastic acrylic resin (DIC 56-1155 in Japan), magnetically stirring for 2h at 500 r/mm, centrifugally dispersing, and ultrasonically washing with 500mL deionized water for 5 times after drying to obtain the chemical grafting modified zinc oxide filler, wherein an electron scanning electron microscope photograph of the chemical grafting modified nano zinc oxide is shown in figure 4.
It can be seen from fig. 4 that the thermoplastic acrylic resin is uniformly grafted on the surface of zinc oxide, and the acrylic resin can slow down the catalytic decomposition of hydrogen peroxide by zinc oxide during storage.
2) Tooth whitening gel and preparation method thereof
(1) Adding 1.5kg of carbomer and 0.8kg of carboxymethyl cellulose into 80.3kg of deionized water, soaking to completely swell, adding 0.3kg of glycerol and 0.1kg of disodium ethylenediamine tetraacetate, and stirring and mixing uniformly to obtain a mixture A1;
(2) Under the stirring condition, adding 12kg of the prepared copper-iron co-doped titanium dioxide nano powder and 0.8kg of coated nano zinc oxide into the mixture A1, and stirring and uniformly mixing to obtain a mixture B1;
(3) 3.5kg of 30% hydrogen peroxide is added into the mixture B1, then 0.12kg of sodium monofluorophosphate, 0.05kg of bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide and 0.03kg of erythromycin are sequentially added, stirring is carried out at room temperature for 4 hours, after uniform mixing, 0.5kg of potassium hydroxide is added to detect the pH value, after the pH value is regulated to 7.0, the thickener is fully thickened, and the mixture C1 is obtained, namely the tooth whitening gel is obtained;
filling the tooth whitening gel into a PVC pipe, and packaging to obtain the visible light tooth whitening gel which can be sold in the market. The obtained visible light tooth whitening gel is suitable for whitening visible light teeth.
The application of the obtained visible light tooth whitening gel is as follows:
100 subjects were selected and randomly divided into two groups, wherein one group of the tooth whitening gel prepared in example 1 was applied during the test, and the other group of the visible light tooth whitening gel was applied during the test;
a1 The tooth whitening gel prepared in example 1 was applied to the teeth of 50 subjects with a thickness of 0.5mm, and was irradiated with light of 460nm wavelength of LED for 30min, once a day, for ten consecutive days, to complete tooth whitening. Compared with untreated teeth, the whitening effect is remarkable, and no uncomfortable symptoms appear.
a2 Taking traditional visible light tooth whitening gel (purchased from Novashine company), respectively smearing the gel on teeth of 50 other subjects, wherein the smearing thickness is 0.5mm, and irradiating the gel for 30min by using the gel with the LED visible light wavelength of 460nm, so that the gel is used once a day for ten continuous days, and tooth whitening is completed. 42 persons produced a remarkable whitening effect compared to untreated persons, and 8 persons did not exhibit tooth whitening effect. Wherein 2 people have symptoms of tooth bleeding and pain, and 2 people have symptoms of eye blooding and dazzling.
The tooth whitening gel of example 2, the preparation method and the application are basically the same as those of example 1, except that the calcination temperature of the nano titanium dioxide powder is 500 ℃, the application process of example 2 is the same as that of example 1, except that the trial results are different, and the detail is shown in table 1, and the electron scanning electron microscope photo of the prepared copper-iron co-doped titanium dioxide is shown in fig. 3, and the morphology is porous spherical, so that the catalytic performance of visible light can be obviously improved.
The tooth whitening gel, the preparation method and the application of the example 3 are basically the same as those of the example 1, except that the resin adopted by the zinc oxide as the whitening filler modified by chemical grafting is high molecular epoxy resin in the preparation process of the whitening gel, and the application process of the example 3 is the same as that of the example 1, except that the trial results are different, and the details are shown in the table 1.
Comparative examples 1-3 tooth whitening gel, preparation method and application
Comparative examples 1 to 2 are a visible light tooth whitening gel, a preparation method and an application, and the steps are basically the same as those of example 1, except that the preparation process parameters of the whitening gel are different, wherein copper-iron co-doped titanium dioxide nano powder is not added in comparative example 1, light stabilizer is not added in comparative example 2, the whitening filler of comparative example 3 is zinc oxide subjected to no chemical grafting modification treatment, and the application process is the same as that of example 1, except that the whitening effect and the hydrogen peroxide concentration in the storage process are different, and the specific details are shown in table 1:
the evaluation of the above-mentioned remarkable tooth whitening effect was performed according to a tooth whiteness color chart, which divides the hundred degrees of teeth into 12 grades altogether, wherein grade 1 is the whitest and grade 12 is the yellowst. The whiteness of the teeth is recorded by photographing the subject before coating the whitening gel, and the whiteness of the teeth is recorded after using the whitening gel for 10 times, and if the whiteness of the teeth is improved by 5 grades or more before and after using, the whiteness is recorded as the remarkable tooth whitening effect of the subject.
It should be noted that the above-mentioned embodiments are merely illustrative of the technical concept and features of the present invention, and it is intended to enable those skilled in the art to understand the present invention and to implement it accordingly, and any person skilled in the art may make any alterations and modifications to the equivalent embodiments without departing from the technical spirit of the present invention, and any simple modifications, equivalent changes and modifications made to the above-mentioned embodiments shall fall within the scope of the present invention as defined by the appended claims.
Claims (3)
1. A single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel is characterized in that: the tooth whitening gel comprises the following components in parts by weight: 10 to 15 parts of copper-iron co-doped nano titanium dioxide, 0.01 to 0.1 part of light stabilizer, 2 to 3 parts of gel, 3 to 9 parts of 30 percent hydrogen peroxide, 0.1 to 2 parts of desensitizer, 0.1 to 0.5 part of auxiliary agent, 0.5 to 1.0 part of whitening filler and 10 to 82 parts of deionized water;
the copper-iron co-doped nano titanium dioxide is prepared by a hydrothermal method to obtain porous spherical copper-iron co-doped nano titanium dioxide;
the whitening filler is obtained by carrying out surface chemical grafting modification on filler substances through organic resin; wherein the filler material is nano zinc oxide;
the light stabilizer comprises the following components in percentage by mass: 1-1: 5 and a light absorber, wherein the antioxidant is bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide, and the light absorber is erythromycin;
the copper-iron co-doped nano titanium dioxide is prepared by dissolving butyl titanate in butanol solution, namely solution A, adding ferric nitrate and copper nitrate solution into concentrated hydrochloric acid solution, namely solution B, dropwise adding the solution B into the solution A under low-speed stirring to form a mixed solution, carrying out hydrothermal reaction on the mixed solution in a reaction kettle at 150-300 ℃ for 8-12 hours, centrifuging, washing, and calcining in a muffle furnace at 500-650 ℃ for 3-4 hours to obtain copper-iron co-doped nano titanium dioxide powder;
the surface chemical grafting modification is to adopt organic resin to carry out chemical grafting modification on the surface of a filler substance in an organic solvent; wherein the organic resin is epoxy resin or acrylic resin;
the organic solvent is one or more of xylene, n-butanol and ethyl acetate;
the mass ratio of the organic resin to the filler substance is 1: 20-1: 50;
the gel is carbomer and carboxymethyl cellulose; the desensitizer is sodium monofluorophosphate; the auxiliary agent is disodium ethylenediamine tetraacetate and glycerol.
2. A method for preparing the single-component low-hydrogen-peroxide-concentration visible light-catalyzed tooth whitening gel according to claim 1, which is characterized in that:
1) Adding the gel into deionized water for soaking, adding an auxiliary agent, and performing ultrasonic dispersion to obtain a mixture A;
2) Adding copper-iron co-doped titanium dioxide into the mixture A, and uniformly stirring to obtain a mixture B;
3) Uniformly dispersing filler substances into an organic solvent, adding organic resin to perform chemical grafting modification on the filler substances, performing centrifugal separation, and cleaning with deionized water to obtain a whitening filler C;
4) Mixing the mixture B with the whitening filler C, adding 30% hydrogen peroxide by mass, uniformly mixing, adding a desensitizer and a light stabilizer, and regulating the pH value by using an alkali solution to obtain a mixture D, thus obtaining the tooth whitening gel.
3. Use of the single component low hydrogen peroxide concentration visible light catalyzed tooth whitening gel of claim 1, wherein: the application of the tooth whitening gel in tooth whitening under photocatalysis.
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| CN202210020205.0A CN114983849B (en) | 2022-01-10 | 2022-01-10 | Single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel and preparation and application thereof |
| PCT/CN2022/090439 WO2023130629A1 (en) | 2022-01-10 | 2022-04-29 | Single-component visible-light-catalyzed teeth whitening gel having low hydrogen peroxide concentration, and preparation and use thereof |
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| CN202210020205.0A CN114983849B (en) | 2022-01-10 | 2022-01-10 | Single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel and preparation and application thereof |
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| CN102614090A (en) * | 2012-04-24 | 2012-08-01 | 苏州维蒂卡科技有限公司 | Toothpaste composition |
| TWI455890B (en) * | 2012-07-09 | 2014-10-11 | Univ Nat Chi Nan | Bimetal modified titanium dioxide and preparation method thereof |
| JP6945810B2 (en) * | 2017-12-22 | 2021-10-06 | 日本メナード化粧品株式会社 | Emulsified cosmetics |
| CN112538303A (en) * | 2020-12-10 | 2021-03-23 | 桐乡市创辉科技合伙企业(有限合伙) | Anti-aging zinc oxide modified acrylic resin wear-resistant coating and preparation method thereof |
| CN113499767B (en) * | 2021-06-21 | 2024-03-15 | 中国科学院海洋研究所 | Visible light catalytic modified titanium dioxide and preparation method and application thereof |
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