Tooth whitening gel and preparation method thereof

Abstract

The invention discloses a tooth whitening gel and a preparation method thereof. The tooth whitening gel comprises the following components in percentage by mass: 5%-25% of a film-forming agent, 0.1%-15% of peroxide, 0.1%-15% of a regulator and 45%-94.8% of a volatile solvent, the film-forming agent is modified ethyl cellulose, and the preparation method comprises the step of treating ethyl cellulose by adopting one or more of irradiation, illumination, oxidation, heating, mechanical pulverization and grinding to obtain the modified ethyl cellulose. The preparation method of the tooth whitening gel comprises the step of uniformly mixing the raw materials including the film-forming agent, the peroxide, the regulator and the volatile solvent to obtain the tooth whitening gel. The tooth whitening gel provided by the invention can be ensured not to be dissolved by saliva after being smeared on teeth, and can be ensured to be completely removed when being removed.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of dental whitening gel, in particular to a tooth whitening gel and a preparation method thereof. BACKGROUND

[0002] In recent years, tooth whitening technology has developed rapidly, and various forms of whitening products have been developed. For example, whitening toothpaste, whitening mouthwash, whitening chewing gum, whitening patches, and tooth whitening gel. High peroxide concentration whitening gel is generally used with a whitening tray, assisted by light or other methods, and low peroxide concentration whitening gel is generally directly applied to the teeth and removed after a period of time. The use is more simple.

[0003] The whitening gel directly applied to the teeth will be eroded and dissolved by saliva, swallowed, low in durability and harmful to health. Accordingly, some reports such as patent specifications with publication numbers CN107635544A, CN114948759A, and CN108348444A all mention dry film-forming whitening gel.

[0004] This whitening gel is mainly composed of hydrophobic film-forming substances and volatile solvents. After being applied to the teeth, the solvent volatilizes to form a stable film, and the peroxide is released for a long time, and it will not be dissolved and eroded by saliva. However, most of the film-forming substances used in these methods are synthetic chemical polymer materials, which have poor biocompatibility. The use of carboxyl as an adhesion group can reduce the pH of the tooth surface, damage the enamel surface, and be difficult to remove after use, leaving white spots on the teeth, which are eventually swallowed and harmful to health.

[0005] The patent specification with publication number CN118236312A discloses a preparation method for a residual-free whitening tooth patch, in which the film-forming agent used is polyvinylpyrrolidone, with a content of 50%~80%, and ethyl cellulose is used as a viscosity reducer, with a content of 0.5%~1%. The patent technology uses ethyl cellulose to cooperate with the gelling agent (one or more of polymethyl methacrylate and methyl methacrylate copolymer, with a content of 2%~5%) in the gel layer to ensure that the tooth patch will not stick to the teeth after use, improving the user's experience. SUMMARY

[0006] The present application provides a tooth whitening gel and a preparation method thereof. The tooth whitening gel of the present application can be used for tooth whitening. When used, it can be directly applied to the teeth, maintained for a period of time, and then removed to whiten the teeth. During use, it will not change the pH of the tooth surface. The tooth whitening gel of the present application can ensure that it is not dissolved by saliva after being applied to the teeth, and can be completely removed when removed.

[0007] The specific technical solution is as follows: In a first aspect, the present application provides a tooth whitening gel, the composition of which comprises, in mass percentage, a film-forming agent 5-25% (e.g. 10%, 13%, 16%, 20%, etc.), a peroxide 0.1-15% (e.g. 1%, 3%, 6%, 10%, etc.), a regulator 0.1-15% (e.g. 0.6%, 1%, 2%, 3%, 3.6%, 4%, etc.), and a volatile solvent 45-94.8% (e.g. 50%, 55%, 60%, 65%, 70%, 75%, 77%, 77.4%, 78%, 80%, 85%, 89.8%, 90%, etc.). The film-forming agent is modified ethyl cellulose, and the preparation method thereof comprises: treating ethyl cellulose by one or more combinations of irradiation, illumination, oxidation, heating, mechanical crushing, and grinding to obtain the modified ethyl cellulose.

[0008] The inventors have found that untreated ethyl cellulose has no adhesion and cannot be used as a single film-forming agent to stabilize the tooth whitening gel on the teeth.

[0009] The present application uses one or more combinations of irradiation, illumination, oxidation, heating, mechanical crushing, and grinding to treat ethyl cellulose, breaks the main chain and / or side chain of ethyl cellulose, changes part of the functional groups, obtains modified ethyl cellulose, and uses the modified ethyl cellulose as a single film-forming agent to make tooth whitening gel.

[0010] Compared with untreated ethyl cellulose, the film-forming agent modified ethyl cellulose of the present application increases some moderate hydrophilicity and adhesion.

[0011] The tooth whitening gel of the present application uses modified ethyl cellulose as a single film-forming agent, has good biocompatibility, and can increase a small amount of hydrophilic groups through irradiation, illumination, oxidation, heating, mechanical crushing, and grinding modification. These hydrophilic groups can ensure that the tooth whitening gel continuously adheres to the tooth surface during use and does not change the pH of the tooth surface, while ensuring that the tooth whitening gel can be completely removed by brushing or other methods after use and does not remain on the tooth surface, and even less likely to be accidentally swallowed.

[0012] In order to better achieve the above-mentioned effects, the composition of the tooth whitening gel preferably comprises, in mass percentage, a film-forming agent 10-25%.

[0013] In some preferred examples, the tooth whitening gel, the number average molecular weight of the ethyl cellulose is greater than 100,000 g / mol, which is conducive to its better use as a single film-forming agent to make the tooth whitening gel with the above-mentioned effects after modification according to the method of the present application.

[0014] In order to achieve the above-mentioned effects, in some preferred examples, the preparation method of the film-forming agent (i.e. the modified ethyl cellulose) comprises: sequentially irradiating and grinding ethyl cellulose to obtain the modified ethyl cellulose.

[0015] In some preferred examples, the irradiation is gamma irradiation, such as cobalt 60 gamma irradiation, etc.

[0016] In some preferred examples, the irradiation dose is 1-40 kGy, such as 20 kGy, etc., and is further preferably 15-25 kGy.

[0017] In some preferred examples, the irradiation time is 0.1-20 hours, such as 3 hours, etc., and is further preferably 2-4 hours.

[0018] In some preferred examples, the grinding is ball milling. Further preferably, the ball milling speed is 250-350 rpm, such as 300 rpm, etc., and the ball milling time is 1.5-2.5 hours, such as 2 hours, etc.

[0019] In some preferred examples, the tooth whitening gel, the peroxide comprises at least one of hydrogen peroxide, urea peroxide, and an aqueous solution containing hydrogen peroxide and / or urea peroxide. Further preferably, the mass percentage of hydrogen peroxide and / or urea peroxide in the aqueous solution containing hydrogen peroxide and / or urea peroxide is 50% or more.

[0020] In some preferred examples, the tooth whitening gel, the volatile solvent can dissolve the film-forming agent. Further preferably, the volatile solvent comprises at least one of ethanol, isopropyl alcohol, ethyl acetate, ethyl butyrate, and n-hexane. More preferably, the volatile solvent comprises ethanol.

[0021] In the present application, the adjusting agent can be a functional auxiliary agent, such as an agent that can improve the physical and chemical properties of the tooth whitening gel after being added.

[0022] In some preferred examples, the tooth whitening gel, the adjusting agent comprises one or more of a thickening agent and a flavoring agent.

[0023] In some preferred examples, the tooth whitening gel, the thickening agent comprises a hydrophobic polymer material.

[0024] In some preferred examples, the tooth whitening gel, the thickening agent preferably comprises at least one of an acrylate copolymer and a vinyl acetate copolymer, and further preferably comprises an acrylate copolymer. More preferably, the acrylate copolymer comprises an acrylic acid (ester) / octyl acrylamide copolymer, and the vinyl acetate copolymer comprises a vinylpyrrolidone-vinyl acetate copolymer.

[0025] In some preferred embodiments, the composition of the tooth whitening gel comprises the thickening agent in an amount of 1% to 15% by mass, for example 3% by mass, etc.

[0026] In some preferred embodiments, the tooth whitening gel comprises a flavoring agent comprising at least one of a sugar and a flavoring essence.

[0027] Further preferably, the sugar comprises at least one of sucralose, xylitol, saccharin, sorbitol, lactitol, and mannitol.

[0028] Further preferably, the flavoring essence comprises at least one of a peppermint flavoring essence, a sweet orange flavoring essence, and a passion fruit flavoring essence. Further preferably, the flavoring essence comprises a peppermint flavoring essence.

[0029] In some preferred embodiments, the composition of the tooth whitening gel comprises the flavoring agent in an amount of 0.1% to 3% by mass, for example 0.6% by mass, 1% by mass, 2% by mass, etc.

[0030] In some preferred embodiments, the tooth whitening gel comprises the film-forming agent, the peroxide, the conditioning agent, and the volatile solvent in a total amount of 100% by mass.

[0031] In some preferred embodiments, the tooth whitening gel has a viscosity of 10 to 1000 cps.

[0032] In a second aspect, the present application provides a method for preparing the tooth whitening gel of the first aspect, comprising: mixing raw materials comprising a film-forming agent, a peroxide, a conditioning agent, and a volatile solvent to obtain the tooth whitening gel.

[0033] In some preferred embodiments, the method for preparing the tooth whitening gel comprises using an excess amount of the volatile solvent during the mixing of the raw materials, and evaporating the volatile solvent after the mixing of the raw materials until the mass of the obtained mixture reaches a desired mass.

[0034] In some preferred embodiments, the method for preparing the tooth whitening gel comprises dissolving the film-forming agent in the volatile solvent to form a uniform solution, and then mixing the solution with the peroxide and the conditioning agent to obtain the tooth whitening gel.

[0035] The tooth whitening gel of the present application has better biocompatibility, is safer to use, and is easier to remove after use.

[0036] Compared with the prior art, the present application has the following beneficial effects: The tooth whitening gel of the present application uses modified ethyl cellulose as a single film-forming agent, which increases the biocompatibility of the tooth whitening gel. By appropriately increasing the hydrophilicity of ethyl cellulose through modification, the problem of ineffective adhesion of untreated pure ethyl cellulose to teeth is solved, while the viscosity is limitedly increased, so that it can be completely removed after use, without residue, reducing the risk of mis-swallowing.

[0037] The present application does not use carboxyl as an adhesion group, so it does not reduce the pH of the tooth surface and damage the enamel surface. Therefore, compared with the prior art, the present application improves safety.

[0038] In addition, the preparation method of the tooth whitening gel of the present application is simple in process, mild in preparation conditions and low in cost. BRIEF DESCRIPTION OF DRAWINGS

[0039] Figure 1 The tooth photographs obtained after in vitro use of the tooth whitening gel, wherein: a figure uses a Crest tooth whitening essence pen; b figure uses the tooth whitening gel of example 1; c figure uses the tooth whitening gel of example 2. DETAILED DESCRIPTION

[0040] The present application will be further described below in conjunction with the drawings and specific examples. It should be understood that these examples are only used to illustrate the present application and not to limit the scope of the present application.

[0041] The operation methods not specified in the following examples are usually carried out according to conventional conditions or according to the conditions recommended by the manufacturers.

[0042] In the following examples: The number average molecular weight of the ethyl cellulose used is greater than 100,000 g / mol; The irradiation used is cobalt 60 gamma ray irradiation.

[0043] Example 1: The target production is 3 kilograms of tooth whitening gel, and the preparation method of the tooth whitening gel comprises the following steps: S1, irradiate the ethyl cellulose, the irradiation dose is 20 kGy, and the irradiation time is 3 hours. Then grind the irradiated ethyl cellulose using a ball mill, the rotation speed of the ball mill is 300 r / min, and the grinding time is 2 hours to obtain modified ethyl cellulose.

[0044] S2, add 480 g of modified ethyl cellulose obtained in step S1 to slightly excessive anhydrous ethanol, stir for 2 hours to dissolve, then add 180 g of 50% mass fraction hydrogen peroxide aqueous solution and 18 g of peppermint essence.

[0045] S3, continue to stir until the mass of the mixture reaches the desired mass of 3 kg, i.e. the desired tooth whitening gel is obtained.

[0046] The composition of the tooth whitening gel of the present embodiment is, in mass percentage, film-forming agent modified ethyl cellulose 16%, volatile solvent ethanol 77.4%, hydrogen peroxide 3%, water 3%, and flavoring agent peppermint essence 0.6%.

[0047] Example 2: The method for preparing the tooth whitening gel comprises the following steps: S1, irradiate the ethyl cellulose at a dose of 20 kGy for 3 hours. Then grind the irradiated ethyl cellulose using a ball mill at a speed of 300 r / min for 2 hours to obtain modified ethyl cellulose.

[0048] S2, add 390 g of the modified ethyl cellulose obtained in step S1 to slightly excessive anhydrous ethanol and stir for 2 hours to dissolve. After dissolution, add 90 g of acrylic acid (ester) / octyl acrylamide copolymer, 180 g of 50% mass fraction hydrogen peroxide aqueous solution, and 18 g of peppermint essence.

[0049] S3, continue to stir until the mass of the mixture reaches the desired mass of 3 kg, i.e. the desired tooth whitening gel is obtained.

[0050] The composition of the tooth whitening gel of the present embodiment is, in mass percentage, film-forming agent modified ethyl cellulose 16%, volatile solvent ethanol 77.4%, hydrogen peroxide 3%, water 3%, and flavoring agent peppermint essence 0.6%.

[0051] The detection method for the in vitro tooth whitening gel removal experiment is introduced as follows: Step 1, take an isolated bovine tooth, clean and dry the tooth surface.

[0052] Step 2, apply the tooth whitening gel to the dried tooth surface, and immediately place it in artificial saliva at 37°C for 4 hours.

[0053] Step 3, after 4 hours, use a toothbrush and toothpaste to simulate normal brushing, and dry the tooth surface.

[0054] Step 4, after drying, take pictures under sufficient light.

[0055] The inventor respectively used the Crest tooth whitening pen and the tooth whitening gel of Example 1 and Example 2 to carry out the above-mentioned in vitro tooth whitening gel use and removal experiment, and after keeping at 37℃ for 4 hours, each tooth whitening gel was intact, indicating that the tooth whitening gel of Example 1 and Example 2 can ensure not to be dissolved by saliva after being applied to the teeth.

[0056] Figure 1 The tooth physical photos obtained after the use and removal of different tooth whitening gels in vitro are shown, wherein: a figure uses the Crest tooth whitening pen; b figure uses the tooth whitening gel of Example 1; c figure uses the tooth whitening gel of Example 2. It can be seen therefrom that the tooth whitening gel of Example 1 and Example 2 can be completely removed when removed, while the existing tooth whitening gel will have more residues, for example Figure 1 There are a large number of white areas on the tooth surface of a in which the existing tooth whitening gel cannot be completely removed.

[0057] Table 1 shows the tooth whitening effect of the tooth whitening gel of Example 2, which is reflected by the color difference of the tooth surface before and after using the tooth whitening gel of Example 2. The use mode is to use it once a day, keep it for 8 hours each time, and continuously use it for 7 days. In Table 1: L, L' represents the lightness, which is the representation of the depth of black and white, and is positive, and the larger the value, the whiter (brighter), and the smaller the value, the darker (darker); a, a', b, b' represent the chroma, specifically, a, a' is the representation of red and green, positive indicates red, negative indicates green, b, b' is the representation of yellow and blue, positive indicates yellow, negative indicates blue; the color difference value ΔE = [(L-L')^2+(a-a')^2+(b-b')^2]^0.5 before and after use.

[0058] Table 1

[0059] As can be seen from Table 1, after using the tooth whitening gel of Example 2, the brightness of the tooth surface is improved and the yellowness is reduced, indicating that the tooth whitening gel of Example 2 has good tooth whitening effect.

[0060] In addition, it should be understood that, after reading the above description of the present application, those skilled in the art can make various modifications or modifications to the present application, and these equivalent forms also fall within the scope defined by the claims attached to the present application.

Claims

1. A teeth whitening gel, characterized in that, By weight percentage, the teeth whitening gel comprises 5%–25% film-forming agent, 0.1%–15% peroxide, 0.1%–15% modifier, and 45%–94.8% volatile solvent; The film-forming agent is modified ethyl cellulose, and its preparation method includes: treating ethyl cellulose by one or more combinations of irradiation, light irradiation, oxidation, heating, mechanical crushing, and grinding to obtain the modified ethyl cellulose.

2. The teeth whitening gel according to claim 1, characterized in that, The number-average molecular weight of the ethyl cellulose is greater than 100,000 g / mol.

3. The teeth whitening gel according to claim 1, characterized in that, The irradiation is gamma-ray irradiation, with an irradiation dose of 1~40 kGy and an irradiation time of 0.1~20 hours.

4. The teeth whitening gel according to claim 1, characterized in that, The grinding process is ball milling, with a milling speed of 250~350 rpm and a milling time of 1.5~2.5 hours.

5. The teeth whitening gel according to claim 1, characterized in that, The peroxide includes at least one of hydrogen peroxide, urea peroxide, and an aqueous solution containing hydrogen peroxide and / or urea peroxide; The volatile solvent can dissolve the film-forming agent, including at least one of ethanol, isopropanol, ethyl acetate, ethyl butyrate, and n-hexane.

6. The teeth whitening gel according to claim 1, characterized in that, The regulator includes one or more of thickeners and flavoring agents.

7. The teeth whitening gel according to claim 6, characterized in that, The thickener includes at least one of acrylate copolymer and vinyl acetate copolymer; The teeth whitening gel comprises 1% to 15% of the thickener by weight percentage.

8. The teeth whitening gel according to claim 6, characterized in that, The flavoring agent includes at least one of sugars and flavorings; The sugars include at least one of sucralose, xylitol, saccharin, sorbitol, lactitol, and mannitol; The flavoring includes at least one of peppermint flavoring, sweet orange flavoring, and passion fruit flavoring; The teeth whitening gel comprises 0.1% to 3% of the flavoring agent by weight percentage.

9. The teeth whitening gel according to claim 1, characterized in that, The viscosity of the teeth whitening gel is 10~1000 cps.

10. The method for preparing the teeth whitening gel according to any one of claims 1 to 9, characterized in that, include: The raw materials, including film-forming agents, peroxides, regulators, and volatile solvents, are mixed to obtain the teeth whitening gel.

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