Multi-whitening material containing composite hydroxyapatite and preparation method of multi-whitening material
By combining modified hydroxyapatite with hydrated silica and using biologically active enzymes, the existing whitening toothpaste has solved the problem of damage and poor stability of tooth enamel, achieving efficient and safe teeth whitening effects.
Patent Information
- Application Number
- CN202411632677.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2024-12-17
AI Technical Summary
Existing whitening toothpastes use special particles or peroxides to cause enamel damage, and have poor chemical stability, high irritation to the oral cavity, and cannot effectively remove pigments on the surface of the teeth, which has poor whitening effect.
The multiple whitening material containing composite hydroxyapatite is used to treat hydroxyapatite by low-temperature plasma active water modification, and ball milling with hydrated silica, combined with biologically active enzymes, and teeth whitening is achieved by chemical and physical friction.
It significantly improves the whitening effect of teeth, enhances the wear resistance and gloss of enamel, reduces damage to gums, and has good stability, safety and effectiveness.
Smart Images

Figure SMS_1
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of dental oral cleaning and relates to a multiple whitening material body containing composite hydroxyapatite and a preparation method thereof. Background Art
[0002] Most existing whitening toothpastes use special particle abrasives or peroxides to achieve whitening effects, but particle abrasives can damage tooth enamel and the tooth surface, making it easier for tooth stains to deposit on the tooth surface. Using peroxide to bleach teeth is fast, but it is irritating to the oral cavity and has certain risks.
[0003] The whitening effect of removing the attachments on the tooth surface by friction is relatively poor, and it will damage the tooth enamel. The effective ingredient peroxide in the chemical method is easy to decompose and has poor stability, which requires a strict toothpaste formula system. Long-term use of stain removal and whitening toothpaste with high friction performance and containing oxides has potential harm to tooth enamel, exposed dentin and gums.
[0004] Hydroxyapatite is widely used in teeth whitening due to its excellent properties. Summary of the invention
[0005] The purpose of the present invention is to provide a multi-whitening material body containing composite hydroxyapatite and a preparation method thereof, wherein the prepared material body has excellent whitening effect.
[0006] The purpose of the present invention can be achieved through the following technical solutions: A multiple whitening material containing composite hydroxyapatite, the multiple whitening material comprising the following raw materials in parts by weight: 10-15 parts of deionized water, 0.2-0.3 parts of saccharin sodium, 2-3 parts of surfactant, 30-35 parts of moisturizer, 0.8-1 parts of thickener, 0.3-0.5 parts of preservative, 0.1-0.2 parts of superoxide dismutase, 0.1-0.2 parts of papain, 0.1-0.2 parts of glucose oxidase, 1-2 parts of menthane carboxamide, 20-30 parts of composite hydroxyapatite, and 0.6-1 parts of regulator; The preparation process of the composite hydroxyapatite is as follows: S1.1. In a high voltage electric field, deionized water is treated with a working frequency of 20-25 kHz and a voltage of 5-9 kV for 2-3 min, and the pH value of the solution is adjusted to 2-4 with lactic acid to prepare low-temperature plasma active water; S1.2, stirring 20 to 35 parts by weight of hydroxyapatite and 70 to 85 parts of low-temperature plasma active water at a speed of 300 to 500 r / min for 2 to 4 hours, and obtaining modified hydroxyapatite after drying; S1.3. Grind the modified hydroxyapatite and modified hydrated silica in a mass ratio of 1:(0.5-1) by a ball mill at a speed of 400 r / min for 3 hours to obtain the composite hydroxyapatite.
[0007] As a preferred technical solution of the present invention, in step S1.3, the preparation process of the modified hydrated silica is as follows: S2.1, adding polyvinyl alcohol to deionized water, controlling the temperature to 80°C, stirring to obtain a polyvinyl alcohol solution with a mass fraction of 10-15%, then adding hydrated silica, stirring at room temperature for 1-2 hours, and obtaining a polyvinyl alcohol-hydrated silica composite; S2.2. Dissolve water-soluble resveratrol in deionized water to obtain a resveratrol solution with a mass fraction of 10-15%, mix a polyvinyl alcohol-hydrated silica complex with a volume ratio of 1:1 with the resveratrol solution, stir at 80-95°C for 2-4 h, and continue heating until completely dry to obtain modified hydrated silica.
[0008] As a preferred technical solution of the present invention, the thickener is one of polyvinyl pyrrolidone, xanthan gum and cellulose gum.
[0009] As a preferred technical solution of the present invention, the moisturizing agent is one or more of sorbitol, polyethylene glycol-8, glycerol and trehalose.
[0010] As a preferred technical solution of the present invention, the surfactant is one of sodium lauroyl sarcosinate and lauryl alcohol.
[0011] As a preferred technical solution of the present invention, the preservative is one of sodium methylparaben and sodium benzoate.
[0012] As a preferred technical solution of the present invention, the regulator is one or more of sodium sulfate, potassium chloride and sodium chloride.
[0013] As a preferred technical solution of the present invention, in step S2.1, the solid-to-liquid ratio of the hydrated silica to the polyvinyl alcohol solution is (1-2): 20 g / mL.
[0014] A method for preparing a multi-whitening material containing composite hydroxyapatite, comprising the following preparation process: S1. Fully mix saccharin sodium, a surfactant and deionized water according to weight, and stir to dissolve to obtain a mixture A; S2, adding a thickener to the moisturizer, mixing and homogenizing for 10-15 minutes, then adding superoxide dismutase, papain and glucose oxidase, stirring at a speed of 250 r / min for 80-100 minutes to obtain a mixture B; S3, mixing mixture A and mixture B, and stirring at a speed of 350 r / min for 60 to 90 min to obtain mixture C; S4. Continue to add composite hydroxyapatite and a regulator into the mixture C, stir for 30 minutes under vacuum conditions, continue to add a preservative and menthanecarboxamide and stir for 5 to 10 minutes, and break the vacuum to obtain the composite hydroxyapatite-containing multiple whitening material.
[0015] As a preferred technical solution of the present invention, the temperature during the preparation process is 40-50°C.
[0016] Hydroxyapatite is an important component of teeth and bones. It can form a protective film on the surface of teeth and replace the calcium lost during tooth demineralization through remineralization, fill the fine scratches on the surface of tooth enamel, and enhance the wear resistance and gloss of tooth enamel. Hydroxyapatite has the characteristics of adsorbing substances such as proteins, amino acids, lipids and dextran. It can effectively absorb bacteria, dental plaque and pigments in the mouth, thereby reducing pigment deposition on the surface of teeth. In addition, hydroxyapatite has moderate hardness and can be used as an abrasive in toothpaste to slightly grind away dirt and pigments on the surface of teeth without hurting the gums.
[0017] Hydroxyapatite is modified by low-temperature plasma active water, which contains rich plasma active components. These components have bactericidal effects and can significantly increase the redox potential and hydroxyl content of the solution. When mixed with hydroxyapatite, low-temperature plasma active water can slightly etch the surface of hydroxyapatite, remove pollutants and defects on the surface of hydroxyapatite, and activate atoms and molecules on the surface of hydroxyapatite. Under the action of plasma active water, functional groups such as hydroxyl and amino groups are introduced into the surface of hydroxyapatite, which can improve the hydrophilicity and biocompatibility of hydroxyapatite.
[0018] In the process of treating hydroxyapatite with low-temperature plasma active water, the active ingredients can remain on the surface of hydroxyapatite during the drying process, and hydroxyapatite has a certain adsorption capacity. These active ingredients contain a large amount of oxidative active substances, which can effectively decompose the pigments on the surface of teeth to achieve the effect of whitening teeth. At the same time, it helps the whitening ingredients to better penetrate into the deep structure of teeth, such as enamel and dentin, so as to more effectively remove the stains and spots hidden deep in these structures. In addition, hydroxyapatite can combine with calcium ions on the surface of teeth to form a protective layer. The combination of the two can clean teeth more comprehensively.
[0019] As an abrasive, hydrated silica's fine particles can effectively remove plaque, stains and pigments on the tooth surface, making the teeth whiter. At the same time, it combines with calcium ions on the tooth surface to form a protective film, reducing damage to the teeth from external stimuli and preventing wear on the tooth surface.
[0020] Hydrated silica has a porous structure. These tiny pores and channels give it a huge specific surface area. After being modified with polyvinyl alcohol, it can increase viscosity and stability, while enhancing the cleaning effect and effectively removing dirt and plaque on the surface of teeth. Water-soluble resveratrol has excellent antioxidant properties, which can remove free radicals and maintain the natural luster of teeth. At the same time, combined with the hydrophilic surfactant polyvinyl alcohol, it can increase the solubility of resveratrol and improve the overall effect of the modified hydrated silica. And because of the presence of polyvinyl alcohol on the surface, it can be evenly dispersed when ball-milled with modified hydroxyapatite.
[0021] Papain is a cleaning ingredient in toothpaste that helps remove plaque and tartar. Superoxide dismutase is an antioxidant ingredient in toothpaste that can remove free radicals in the mouth and protect teeth from oxidative damage. Glucose oxidase is also an antioxidant or whitening ingredient in toothpaste that can catalyze glucose to produce gluconolactone and hydrogen peroxide in the presence of oxygen, thereby achieving a whitening effect. By adding three enzyme active ingredients, the bacteria in dental plaque are effectively dissolved by enzymes, breaking down the structure of dental plaque so that it is easy to remove, thereby achieving the effect of whitening teeth.
[0022] Beneficial effects of the present invention: The present invention modifies hydroxyapatite with low-temperature plasma active water, utilizes the active ingredients rich in hydroxyapatite to improve the whitening effect of hydroxyapatite, and simultaneously uses hydrated silica as a friction aid, is treated with a polyvinyl alcohol solution, and is mixed with water-soluble resveratrol having antioxidant properties. The good film-forming property of polyvinyl alcohol and the improvement of the solubility of resveratrol as a hydrophilic surfactant are utilized, so that the water-soluble resveratrol can stably coexist with hydrated silica, the composite hydroxyapatite obtained by ball milling the modified hydroxyapatite and the modified hydrated silica is mixed with other additives, and the biological mode of bioactive enzymes is utilized, and the chemical and physical friction modes are combined to jointly improve the whitening effect through these three modes. DETAILED DESCRIPTION
[0023] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the specific implementation methods, structures, features and effects of the present invention are described in detail below in combination with the embodiments.
[0024] In the following examples and comparative examples: Hydroxyapatite: purchased from Shanghai Kanglang Biotechnology Co., Ltd., product number: KL811001; Polyvinyl alcohol: purchased from Shanghai Myrel Biochemical Technology Co., Ltd., catalog number: N07802; Hydrated silica: purchased from Beijing Lingbao Technology Co., Ltd.; Water-soluble resveratrol: purchased from Fufeng Sinuote Biotechnology Co., Ltd.; Saccharin sodium: purchased from Shanghai Huichu Chemical Technology Co., Ltd.; Sodium lauroyl sarcosinate: purchased from Tesco Chemical (Hubei) Co., Ltd.; Sorbitol: purchased from Shandong Yaheng Biotechnology Co., Ltd.; Polyvinyl pyrrolidone: purchased from Hefei Hongrui Biotechnology Co., Ltd.; Superoxide dismutase: purchased from Shanghai Huicheng Biotechnology Co., Ltd. Papain: purchased from Jiangsu Jiujia Biotechnology Co., Ltd.; Glucose oxidase: purchased from Shaanxi Runfeng Biotechnology Co., Ltd.; Sodium sulfate: purchased from Jiangsu Kolondo Food Ingredients Co., Ltd.; Cellulose gum: purchased from Anhui Runtai Biotechnology Co., Ltd.; Polyethylene glycol-8: purchased from Hubei Chenghai Chemical Co., Ltd.
[0025] Example 1
[0026] Preparation of composite hydroxyapatite: S1.1. In a high voltage electric field, deionized water was treated with a voltage of 5 kV at a working frequency of 20 kHz for 2 min, and the pH value of the solution was adjusted to 2 with lactic acid to prepare low-temperature plasma active water; S1.2, 20 parts by weight of hydroxyapatite and 70 parts of low-temperature plasma active water were stirred at a speed of 300 r / min for 2 h, and the modified hydroxyapatite was obtained after drying; S1.3. Grind the modified hydroxyapatite and the modified hydrated silica in a mass ratio of 1:0.5 by a ball mill at a speed of 400 r / min for 3 hours to obtain the composite hydroxyapatite.
[0027] Preparation of modified hydrated silica: S2.1. Add polyvinyl alcohol to deionized water, control the temperature to 80°C, stir to obtain a polyvinyl alcohol solution with a mass fraction of 10%, then add hydrated silica, stir at room temperature for 1 hour, and obtain a polyvinyl alcohol-hydrated silica composite, wherein the solid-liquid ratio of hydrated silica to polyvinyl alcohol solution is 1:20 g / mL; S2.2. Dissolve water-soluble resveratrol in deionized water to obtain a resveratrol solution with a mass fraction of 10%, mix the polyvinyl alcohol-hydrated silica complex with a volume ratio of 1:1 with the resveratrol solution, stir at 80°C for 2h, and continue heating until completely dry to obtain modified hydrated silica.
[0028] Preparation of multi-whitening material containing composite hydroxyapatite: The temperature during the preparation process was 40°C.
[0029] S1. By weight, 0.2 parts of saccharin sodium, 2 parts of sodium lauroyl sarcosinate and 10 parts of deionized water were fully mixed and stirred to dissolve to obtain a mixture A; S2, adding 0.8 parts of polyvinyl pyrrolidone to 30 parts of sorbitol, mixing and homogenizing for 10 minutes, then adding 0.1 parts of superoxide dismutase, 0.1 parts of papain and 0.1 parts of glucose oxidase, stirring at a speed of 250 r / min for 80 minutes to obtain a mixture B; S3, mixing mixture A and mixture B, and stirring at a speed of 350 r / min for 60 min to obtain mixture C; S4. Continue to add 20 parts of composite hydroxyapatite and 0.6 parts of sodium sulfate to the mixture C, stir for 30 minutes under vacuum conditions, continue to add 0.3 parts of sodium methylparaben and 1 part of menthanecarboxamide and stir for 5 minutes, break the vacuum to obtain the multiple whitening material containing composite hydroxyapatite.
[0030] Example 2
[0031] Preparation of composite hydroxyapatite: S1.1. In a high voltage electric field, deionized water was treated with a voltage of 8 kV at a working frequency of 22.5 kHz for 2.5 min, and the pH value of the solution was adjusted to 3 with lactic acid to prepare low-temperature plasma active water; S1.2, 28 parts by weight of hydroxyapatite and 78 parts of low-temperature plasma active water were stirred at a speed of 400 r / min for 3 h, and modified hydroxyapatite was obtained after drying; S1.3. Grind the modified hydroxyapatite and modified hydrated silica in a mass ratio of 1:0.7 in a ball mill at a speed of 400 r / min for 3 hours to obtain the composite hydroxyapatite.
[0032] Preparation of modified hydrated silica: S2.1. Add polyvinyl alcohol to deionized water, control the temperature to 80°C, stir to obtain a polyvinyl alcohol solution with a mass fraction of 13%, then add hydrated silica, stir at room temperature for 1.5 hours, and obtain a polyvinyl alcohol-hydrated silica composite, wherein the solid-liquid ratio of hydrated silica to polyvinyl alcohol solution is 1.5:20 g / mL; S2.2. Dissolve water-soluble resveratrol in deionized water to obtain a resveratrol solution with a mass fraction of 13%, mix the polyvinyl alcohol-hydrated silica complex with a volume ratio of 1:1 with the resveratrol solution, stir at 88°C for 3 hours, and continue heating until completely dry to obtain modified hydrated silica.
[0033] Preparation of multi-whitening material containing composite hydroxyapatite: The temperature during the preparation process was 45°C.
[0034] S1. By weight, 0.25 parts of saccharin sodium, 2.5 parts of sodium lauroyl sarcosinate and 13 parts of deionized water were fully mixed and stirred to dissolve to obtain a mixture A; S2, adding 0.9 parts of cellulose gum to 33 parts of sorbitol, mixing and homogenizing for 13 minutes, then adding 0.15 parts of superoxide dismutase, 0.15 parts of papain and 0.15 parts of glucose oxidase, stirring at a speed of 250 r / min for 90 minutes to obtain a mixture B; S3, mixing mixture A and mixture B, and stirring at a speed of 350 r / min for 70 min to obtain mixture C; S4. Continue to add 25 parts of composite hydroxyapatite and 0.8 parts of sodium sulfate to the mixture C, stir for 30 minutes under vacuum conditions, continue to add 0.4 parts of sodium methylparaben and 1.5 parts of menthanecarboxamide and stir for 8 minutes, break the vacuum to obtain the composite hydroxyapatite-containing multiple whitening material.
[0035] Example 3
[0036] Preparation of composite hydroxyapatite: S1.1. In a high voltage electric field, deionized water was treated with a voltage of 9 kV at a working frequency of 25 kHz for 3 min, and the pH value of the solution was adjusted to 4 with lactic acid to prepare low-temperature plasma active water; S1.2, 35 parts by weight of hydroxyapatite and 85 parts of low-temperature plasma active water were stirred at a speed of 500 r / min for 4 hours, and the modified hydroxyapatite was obtained after drying; S1.3. Grind the modified hydroxyapatite and the modified hydrated silica in a mass ratio of 1:1 by a ball mill at a speed of 400 r / min for 3 hours to obtain the composite hydroxyapatite.
[0037] Preparation of modified hydrated silica: S2.1. Add polyvinyl alcohol to deionized water, control the temperature to 80°C, stir to obtain a polyvinyl alcohol solution with a mass fraction of 15%, then add hydrated silica, stir at room temperature for 2 hours, and obtain a polyvinyl alcohol-hydrated silica composite, wherein the solid-liquid ratio of hydrated silica to polyvinyl alcohol solution is 2:20 g / mL; S2.2. Dissolve water-soluble resveratrol in deionized water to obtain a resveratrol solution with a mass fraction of 15%, mix the polyvinyl alcohol-hydrated silica complex with a volume ratio of 1:1 with the resveratrol solution, stir at 95°C for 4 h, and continue heating until completely dry to obtain modified hydrated silica.
[0038] Preparation of multi-whitening material containing composite hydroxyapatite: The temperature during the preparation process was 40~50℃.
[0039] S1. By weight, 0.3 parts of saccharin sodium, 3 parts of sodium lauroyl sarcosinate and 15 parts of deionized water were fully mixed and stirred to dissolve to obtain a mixture A; S2, adding 1 part of polyvinyl pyrrolidone to 35 parts of polyethylene glycol-8, mixing and homogenizing for 15 minutes, then adding 0.2 parts of superoxide dismutase, 0.2 parts of papain and 0.2 parts of glucose oxidase, stirring at a speed of 250 r / min for 100 minutes to obtain a mixture B; S3, mixing mixture A and mixture B, and stirring at a speed of 350 r / min for 90 min to obtain mixture C; S4. Continue to add 30 parts of composite hydroxyapatite and 1 part of sodium sulfate to the mixture C, stir for 30 minutes under vacuum conditions, continue to add 0.5 parts of sodium hydroxybenzoate and 2 parts of menthanecarboxamide and stir for 10 minutes, break the vacuum to obtain the composite hydroxyapatite-containing multiple whitening material.
[0040] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that in Comparative Example 1, the hydroxyapatite is not modified by low-temperature plasma active water, and the other operations are the same.
[0041] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that in Comparative Example 2, no water-soluble resveratrol is added to the modified hydrated silica, and the other operations are the same.
[0042] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that polyvinyl alcohol is not used in the preparation of the modified hydrated silica in Comparative Example 3, and the other operations are the same.
[0043] Comparative Example 4 The difference between Comparative Example 4 and Example 1 is that the hydrated silica in Comparative Example 4 is not modified in any way, and the other operations are the same.
[0044] Comparative Example 5 The difference between Comparative Example 5 and Example 1 is that in Comparative Example 5: hydroxyapatite and hydrated silica in a mass ratio of 1:0.5 are ground by a ball mill at a speed of 400 r / min for 3 hours to obtain the composite hydroxyapatite, and the other operations are the same.
[0045] Performance Testing The material prepared by the present invention can be directly used as toothpaste.
[0046] 1. Preparation of dental grinding blocks: Cut bovine incisors into enamel blocks of approximately 5 mm x 5 mm x 2 mm in size, embed them in polymethyl methacrylate resin, grind the enamel labial surface with 180-grit sandpaper moistened with water, and grind the enamel surface of the arc structure flat. Rinse the sample with water, then grind the enamel surface smooth with 600-grit sandpaper moistened with water, and wash it with deionized water in an ultrasonic bath for 15 min.
[0047] 2. Acid etching: immerse the tooth grinding block in 1% hydrochloric acid, stir for 60 seconds, take out and rinse with clean water; then immerse it in saturated sodium carbonate solution, stir for 60 seconds, take out and rinse with clean water; finally immerse it in 1% phytic acid solution, stir for 60 seconds, take out and rinse with clean water.
[0048] 3. Preparation of staining solution: First, dissolve gastric mucin with hot water, then add coffee, soy sauce, and black tea and stir evenly, let smoke pass, let it cool, and add FeCl3 solution stored at 4℃ before use. The final concentration of each component is: gastric mucin 2.5g / L, coffee 4.0g / L, soy sauce 4.0g / L, black tea 4.0g / L, cigarette smoke 4 / L, ferric chloride 0.05g / L.
[0049] 4. Staining of tooth abrasive blocks: Place the acid-etched tooth abrasive blocks in a staining machine for staining for 12 days. Number and mark the stained tooth abrasive blocks, and measure the color of the tooth enamel (L 前 ), that is, L value is the color value of tooth enamel shown by colorimeter, tooth grinding blocks with L value of 30-50 were selected and randomly allocated to sample group and control group, 8 blocks in each group, and there was no significant difference between the groups. The tooth grinding blocks were brushed with toothpaste of embodiment group and comparative example group respectively.
[0050] 5. Preparation of test sample slurry: Weigh a certain weight of the toothpaste to be tested and deionized water in a ratio of 1:1.6 (toothpaste: water), stir with a glass rod to disperse the toothpaste, and then stir with a magnetic stirrer to form a homogenous slurry for later use.
[0051] 6. Simulate the toothbrushing process: Place the tooth grinding block in the sample fixing slot of the automatic mechanical toothbrushing machine and fix it so that the tooth block is about 2mm higher. Tighten the screws to fix it. Install the toothbrush head so that the bristles are in vertical contact with the enamel surface. The total weight of the toothbrush head and rod is 150g. Weigh about 70g of the sample slurry to be tested and add it to the grinding liquid bottle. Fix the grinding liquid bottle on the toothbrushing machine so that the slurry buries the tooth block. Brush your teeth back and forth 800 times. After brushing, remove the tooth grinding block from the toothbrushing machine, rinse it with water, dry it with a paper towel, and dry it.
[0052] 7. Determine the L value of tooth enamel after brushing (L 后 ) and calculate the difference between the L values before and after brushing your teeth △L=L 后 -L 前 .
[0053] 8. Evaluation Method If the ΔL value of the example group is greater than the ΔL value of the comparative example group and there is a significant difference (P<0.05), it can be considered that the teeth in the sample group have the effect of removing exogenous stains. The results are as follows:
[0054] SPSS 27.0 statistical software was used to conduct an independent t test with a test level of α=0.05. The ΔL values of the embodiment group and the comparative example group showed significant differences (P<0.001). At the same time, the ΔL values of the embodiment group were higher than those of the comparative example group. Therefore, the material prepared by the present invention has an excellent whitening effect.
[0055] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A multi-whitening material containing composite hydroxyapatite, It is characterized in that The multiple whitening material comprises the following raw materials in parts by weight: 10-15 parts of deionized water, 0.2-0.3 parts of saccharin sodium, 2-3 parts of surfactants, 30-35 parts of moisturizers, 0.8-1 parts of thickeners, 0.3-0.5 parts of preservatives, 0.1-0.2 parts of superoxide dismutase, 0.1-0.2 parts of papain, 0.1-0.2 parts of glucose oxidase, 1-2 parts of menthane carboxamide, 20-30 parts of composite hydroxyapatite, and 0.6-1 parts of regulators; The preparation process of the composite hydroxyapatite is as follows: S1.
1. In a high voltage electric field, deionized water is treated with a working frequency of 20-25 kHz and a voltage of 5-9 kV for 2-3 min, and the pH value of the solution is adjusted to 2-4 with lactic acid to prepare low-temperature plasma active water; S1.2, 20 to 35 parts by weight of hydroxyapatite and 70 to 85 parts of low-temperature plasma active water are stirred at a speed of 300 to 500 r / min for 2 to 4 hours, and then dried to obtain modified hydroxyapatite; S1.
3. Grind the modified hydroxyapatite and modified hydrated silica in a mass ratio of 1:(0.5-1) by a ball mill at a speed of 400 r / min for 3 hours to obtain the composite hydroxyapatite.
2. The multi-whitening material containing composite hydroxyapatite according to claim 1, It is characterized in that In step S1.3, the preparation process of the modified hydrated silica is as follows: S2.1, adding polyvinyl alcohol to deionized water, controlling the temperature to 80°C, stirring to obtain a polyvinyl alcohol solution with a mass fraction of 10-15%, then adding hydrated silica, stirring at room temperature for 1-2 hours, and obtaining a polyvinyl alcohol-hydrated silica composite; S2.
2. Dissolve water-soluble resveratrol in deionized water to obtain a resveratrol solution with a mass fraction of 10-15%, mix a polyvinyl alcohol-hydrated silica complex with a volume ratio of 1:1 with the resveratrol solution, stir at 80-95°C for 2-4 h, and continue heating until completely dry to obtain modified hydrated silica.
3. The multi-whitening material containing composite hydroxyapatite according to claim 1, It is characterized in that The thickener is one of polyvinyl pyrrolidone, xanthan gum and cellulose gum.
4. The multi-whitening material containing composite hydroxyapatite according to claim 1, It is characterized in that The moisturizing agent is one or more of sorbitol, polyethylene glycol-8, glycerol and trehalose.
5. The multi-whitening material containing composite hydroxyapatite according to claim 1, It is characterized in that The surfactant is one of sodium lauroyl sarcosinate and lauryl alcohol.
6. The multi-whitening material containing composite hydroxyapatite according to claim 1, It is characterized in that The preservative is one of sodium methylparaben and sodium benzoate.
7. The multi-whitening material containing composite hydroxyapatite according to claim 1, It is characterized in that The regulator is one or more of sodium sulfate, potassium chloride and sodium chloride.
8. The multi-whitening material containing composite hydroxyapatite according to claim 2, It is characterized in that In step S2.1, the solid-liquid ratio of the hydrated silica to the polyvinyl alcohol solution is (1-2): 20 g / mL.
9. A method for preparing a multi-whitening material containing composite hydroxyapatite according to any one of claims 1 to 8, It is characterized in that The preparation process includes the following: S1. Fully mix saccharin sodium, a surfactant and deionized water according to weight, and stir to dissolve to obtain a mixture A; S2, adding a thickener to the moisturizer, mixing and homogenizing for 10-15 minutes, then adding superoxide dismutase, papain and glucose oxidase, stirring at a speed of 250 r / min for 80-100 minutes to obtain a mixture B; S3, mixing mixture A and mixture B, and stirring at a speed of 350 r / min for 60 to 90 min to obtain mixture C; S4. Continue to add composite hydroxyapatite and a regulator into the mixture C, stir for 30 minutes under vacuum conditions, continue to add a preservative and menthanecarboxamide and stir for 5 to 10 minutes, and break the vacuum to obtain the composite hydroxyapatite-containing multiple whitening material.
10. The method for preparing the multi-whitening material containing composite hydroxyapatite according to claim 9, It is characterized in that The temperature during the preparation process is 40-50°C.
Citation Information
Patent Citations
Mouth wash containing bio-enzyme composition and preparation method thereof
CN104490621A
Bacterium removal toothpaste
CN106420439A
Mouthwash for inhibiting bacteria, preventing caries and refreshing breath, and preparation method thereof
CN108685773A
High-voltage electric field low-temperature plasma active water continuous generation device
CN111470593A
Whitening toothpaste and preparation method thereof
CN113813196A
