阅读说明：本技术 一种由蓝光led激发的美白牙膏及其制备方法 (Whitening toothpaste excited by blue light LED and preparation method thereof ) 是由 王小磊 辛洪波 余芬 廖岚 张凤 于 2017-08-03 设计创作，主要内容包括：本发明提供了一种由蓝光LED激发的美白牙膏及其制备方法,该技术方案以二氧化钛,盐酸多巴胺,六次亚甲基四胺为主要原料,混合后与六次亚甲基四胺反应,产物经洗涤、干燥后得到成品。该牙膏产品以二氧化钛为主体美白剂,能够在蓝光的激发下对变色牙快速产生氧化还原反应,同时还具有如下技术优势：1、能够响应可见光,不需要通过紫外激发即可发生氧化还原作用,更为健康安全。2、工艺简单安全,无需添加有机溶剂,操作方法简单,对设备要求不高,适用于大规模生产及工业化推广。(The invention provides a whitening toothpaste excited by a blue light LED and a preparation method thereof. The toothpaste product takes titanium dioxide as a main whitening agent, can quickly generate oxidation-reduction reaction on discolored teeth under the excitation of blue light, and simultaneously has the following technical advantages: 1. can respond to visible light, can generate oxidation-reduction action without ultraviolet excitation, and is more healthy and safe. 2. The method has the advantages of simple and safe process, no need of adding organic solvent, simple operation method, low requirement on equipment and suitability for large-scale production and industrial popularization.)

1. The whitening toothpaste excited by the blue light LED is characterized in that the visible light is blue light with the wavelength of 450-480 nm, and the toothpaste contains 3-8% of polydopamine-coated titanium dioxide by mass.

2. The whitening toothpaste excited by a blue light LED according to claim 1, wherein the toothpaste contains 5% by weight of polydopamine-coated titanium dioxide.

3. The method of preparing whitening toothpaste excited by blue LED according to claim 1, comprising the steps of:

1) sequentially adding 0.06-0.10g of nano titanium dioxide and 0.009-0.011g of dopamine hydrochloride into 48-52mL of pure water and uniformly mixing to obtain an aqueous solution;

2) adding hexamethylenetetramine into the aqueous solution obtained in the step 1), ultrasonically oscillating for 5min, sealing the container, and then carrying out water bath at 88-92 ℃ for 2.5-3.5 h; the addition amount of the hexamethylene tetramine is 9-11 times of the weight of the dopamine hydrochloride in the step 1);

3) washing the product obtained in the step 2), and freeze-drying to obtain the whitening toothpaste with visible light excited redox reaction.

4. The preparation method of the whitening toothpaste excited by the blue light LED as claimed in claim 3, wherein the amount of the nano titanium dioxide, the dopamine hydrochloride and the pure water in the step 1) is 0.08g to 0.01g to 50 mL.

5. The preparation method of the whitening toothpaste excited by the blue light LED as claimed in claim 3, wherein the water bath temperature in the step 2) is 90 ℃ and the water bath time is 3h in the step 1); the addition amount of the hexamethylene tetramine is 10 times of the weight of the dopamine hydrochloride in the step 1).

6. The method for preparing the whitening toothpaste excited by the blue light LED according to claim 3, wherein the washing in the step 3) is that the product obtained in the step 2) is washed with pure water for 2-3 times, then washed with absolute ethyl alcohol for 2-3 times, and then washed with pure water for 2-3 times.

Technical Field

The invention relates to the technical field of toothpaste preparation, and simultaneously relates to the technical field of tooth whitening, in particular to whitening toothpaste excited by blue light LEDs and a preparation method thereof

Background

Since the color and luster of teeth directly affect the facial appearance, tooth whitening has become a general cosmetic requirement, and with the development of medical technology, a variety of restoration means for discolored teeth have been developed in recent years, wherein the applications of covering whitening and chemical bleaching are common. The main methods of masking and whitening include veneering and full crown restoration, both of which require extensive grinding of the tooth and thus irreversible damage to the structure of the tooth itself. The chemical bleaching method is relatively safe, but depends on chemical reaction, so the reaction design is very important, and if the reactant components are not reasonable, the whitening effect is not ideal, and even side effects can be generated.

The method is characterized in that high-intensity blue light with the wavelength of 480-520 nm irradiates a reagent with hydrogen peroxide or carbamide peroxide as a main component to generate an oxidation-reduction reaction, and pigments attached to the surface and the deep layer of a tooth are removed through dentinal tubules, so that the whitening effect is achieved. Although this method has shown a good tooth-cleaning effect, there are side effects such as enamel demineralization, soft tissue irritation, tooth sensitivity, acute pulpitis, etc. in practical use because the reactive components are not safe enough. Therefore, how to provide a whitening toothpaste which is catalyzed by mild light and has safe and effective ingredients is a technical problem which needs to be solved urgently by the technical personnel in the field.

Disclosure of Invention

The invention aims to provide whitening toothpaste excited by a blue light LED and a preparation method thereof aiming at overcoming the technical problems that in the prior art, teeth are bleached by photocatalytic oxidation reaction, the whitening effect is poor due to unreasonable reactant design, and tooth enamel is damaged.

In order to achieve the technical purpose, the invention adopts the following technical scheme:

the whitening toothpaste excited by the blue light LED is characterized in that the visible light is blue light with the wavelength of 450-480 nm, and the toothpaste contains 3-8% of polydopamine-coated titanium dioxide by mass.

Preferably, the toothpaste contains 5% of polydopamine-coated titanium dioxide by mass.

The invention utilizes polydopamine to coat and modify the surface of titanium dioxide nano particles, so that electrons are excited to generate active oxygen with strong oxidizing property under the condition of visible light and blue light, and pigments are decomposed by oxidation-reduction reaction, thereby achieving the effect of whitening teeth. Meanwhile, titanium dioxide coated by polydopamine in the invention is neutral and alkaline, has low cytotoxicity and no corrosivity, and hardly damages enamel surface structures.

A preparation method of whitening toothpaste excited by a blue light LED comprises the following steps:

1) sequentially adding 0.06-0.10g of nano titanium dioxide and 0.009-0.011g of dopamine hydrochloride into 48-52mL of pure water and uniformly mixing to obtain an aqueous solution;

2) adding hexamethylenetetramine into the aqueous solution obtained in the step 1), ultrasonically oscillating for 5min, sealing the container, and then carrying out water bath at 88-92 ℃ for 2.5-3.5 h; the addition amount of the hexamethylene tetramine is 9-11 times of the weight of the dopamine hydrochloride in the step 1);

3) washing the product obtained in the step 2), and freeze-drying to obtain the whitening toothpaste excited by the visible light for oxidation and reduction reaction.

Preferably, the dosage of the nano titanium dioxide, the dopamine hydrochloride and the pure water in the step 1) is 0.08g to 0.01g to 50 mL.

Preferably, the water bath temperature in the step 2) in the step 1) is 90 ℃, and the water bath time is 3 hours; the addition amount of the hexamethylene tetramine is 10 times of the weight of the dopamine hydrochloride in the step 1).

Preferably, the washing in step 3) is washing the product obtained in step 2) with pure water for 2-3 times, then washing with absolute ethyl alcohol for 2-3 times, and then washing with pure water for 2-3 times.

Preferably, the container in step 1) is a conical flask.

Preferably, the toothpaste can be directly dissolved in water for use, and can also be prepared into gel, paste and the like by adding pharmaceutical excipients.

In the above technical scheme, the visible light-excited redox reaction is a photocatalytic reaction, and specifically belongs to an oxidation reaction catalyzed by visible light.

The invention provides a whitening toothpaste excited by a blue light LED and a preparation method thereof. Pure nano TiO₂Is a wide forbidden band semiconductor, has low utilization rate to visible light, and uses PDA to nano TiO₂Coating the surface of the particle to form nano TiO₂The @ PDA compound, and then make the product can produce redox reaction to the tooth that becomes colour under the excitation of blue light fast, still have following technological advantage simultaneously:

1. the ultraviolet-light-emitting material can respond to visible light blue light, can generate redox effect without ultraviolet excitation, and is more healthy and safe.

2. The method has the advantages of simple and safe process, no need of adding organic solvent, simple operation method, low requirement on equipment and suitability for large-scale production and industrial popularization.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.

FIG. 1 shows the nano TiO compound obtained in example 1 of the present invention₂TEM scan of @ PDA, where FIG. 1C is its SEAD plot in the upper right corner;

FIG. 2 shows the nano TiO compound obtained in example 1 of the present invention₂The EDS map of @ PDA;

FIG. 3 shows a view of nano TiO₂The nano TiO obtained in examples 1 to 3 of the present invention₂XRD patterns of @ PDA and PDA;

FIG. 4 shows a view of nano TiO₂The nano TiO obtained in examples 1 to 3 of the present invention₂@ PDA and PDA ultraviolet absorption spectrograms;

FIG. 5 is a graph showing the results of an experiment in example 6 of the present invention; wherein, parts A-F are graphs of whitening effects of the toothpaste prepared in example 1 on experimental teeth after treatment for different action times, respectively; fig. 5G is a chart of the whitening color gradation of the dental professional colorimetric card;

FIG. 6 is a scanning electron micrograph of experimental tooth enamel after 0.5h of treatment without treatment and using the method described in example 6;

FIG. 7 is a scanning electron micrograph of experimental tooth enamel after 4h treatment without treatment and using the method described in example 6;

FIG. 8 is a scanning electron micrograph of experimental tooth enamel after 0.5h of treatment without treatment and using the method described in comparative example 1;

FIG. 9 is a scanning electron micrograph of Staphylococcus aureus on teeth in test example 1.

FIG. 10 is a graph showing the results of the agar counting plate in test example 2.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The embodiment of the invention provides whitening toothpaste excited by a blue light LED, visible light is blue light with the wavelength of 450-480 nm, and the toothpaste contains 3-8% of polydopamine-coated titanium dioxide by mass.

Preferably, the toothpaste contains 5% of polydopamine-coated titanium dioxide by mass.

The embodiment of the invention also provides a preparation method of the whitening toothpaste excited by the blue light LED, which comprises the following steps:

1) sequentially adding 0.06-0.10g of nano titanium dioxide and 0.009-0.011g of dopamine hydrochloride into 48-52mL of pure water and uniformly mixing to obtain an aqueous solution;

2) adding hexamethylenetetramine into the aqueous solution obtained in the step 1), ultrasonically oscillating for 5min, sealing the container, and then carrying out water bath at 88-92 ℃ for 2.5-3.5 h; the addition amount of the hexamethylene tetramine is 9-11 times of the weight of the dopamine hydrochloride in the step 1);

3) washing the product obtained in the step 2), and freeze-drying to obtain the whitening toothpaste excited by the visible light for oxidation-reduction reaction.

In order to further optimize the technical scheme of the invention, the dosage of the nano titanium dioxide, the dopamine hydrochloride and the pure water in the step 1) is 0.08g to 0.01g to 50 mL.

Further, in the step 2), the water bath temperature in the step 1) is 90 ℃, and the water bath time is 3 hours; the addition amount of hexamethylenetetramine is 10 times of the weight of dopamine hydrochloride in the step 1).

Further, in the step 3), the product obtained in the step 2) is washed with pure water for 2-3 times, then washed with absolute ethyl alcohol for 2-3 times, and then washed with pure water for 2-3 times.

Further, the container in the step 1) is a conical flask.

Furthermore, the toothpaste can be directly dissolved in water for use, or can be made into gel, paste, ointment, etc. by adding medicinal adjuvants.

The technical solution of the present invention is further illustrated by the following specific embodiments, and the approximating language used in the following embodiments may be applied for quantitative representation, indicating that certain changes may be made in the allowable amount without changing the basic function. Accordingly, a numerical value modified by a language such as "about", "left or right" is not limited to the precise numerical value itself. In some embodiments, "about" indicates that the value allowed for correction varies within plus or minus ten percent (10%), for example, "about 100" indicates that any value between 90 and 110 is possible. Further, in the expression "about a first value to a second value", both the first and second values are corrected at about the same time. In some cases, the approximating language may be related to the precision of a measuring instrument.