Tooth whitening composition with good storage stability and preparation method thereof

Abstract

The invention discloses a tooth whitening composition with good storage stability and a preparation method thereof. The tooth whitening composition comprises 60-70% of a hydrogen peroxide solution, 0.1-10% of micromolecular organic amine, 0.1-5% of a nonionic surfactant, 1-10% of a stabilizer, 4-6% of a thickener, 0.1-0.2% of essence, 10-15% of glycerin and the balance of water. Stirring and dissolving hydrogen peroxide, a stabilizer, water, glycerol and micromolecular organic amine to obtain a mixed solution; adding essence and a thickening agent into the mixed solution, and stirring at a high stirring speed of 1000-2000rpm for 5 minutes; the preparation method of the tooth whitening composition comprises the following steps: adding a nonionic surfactant into a reaction kettle, dropwise adding the nonionic surfactant in a stirring state until the nonionic surfactant is completely added, and stirring at a high stirring speed of 1000-2000rpm for 5 minutes to obtain the tooth whitening composition with good storage stability. According to the invention, a stabilizing agent combination scheme taking micromolecular organic amine with a steric hindrance effect as a core is adopted, so that the storage stability of the peroxide-containing tooth whitening product is remarkably improved.

Description

Technical Field

[0001] This invention relates to the field of teeth whitening compositions, and more particularly to a teeth whitening composition with good storage stability and a method for preparing the same. Background Technology

[0002] Teeth whitening methods mainly include chemical bleaching with medications, cover-up whitening, and professional teeth cleaning and air polishing to restore the natural color of teeth. With the increasing development of cosmetic dentistry, chemical bleaching methods containing peroxides are becoming more and more popular. This method uses the redox chemical reaction of peroxides to break down the large organic staining molecules on the tooth surface into smaller molecules, thus lightening the color and fading the pigments deposited on the surface and deep layers of the teeth, achieving teeth whitening. The most commonly used effective chemical components for teeth whitening are hydrogen peroxide or urea peroxide. Urea peroxide is a compound formed by hydrogen bonds between hydrogen peroxide and urea, but its core effective component is still hydrogen peroxide.

[0003] Hydrogen peroxide is a reactive strong oxidant that easily decomposes into water and oxygen. Teeth whitening products containing hydrogen peroxide will continue to decompose from the moment they are manufactured. If affected by various factors such as temperature, metal ion contamination, alkaline environment, and light, the decomposition reaction will be further accelerated. Therefore, teeth whitening products containing hydrogen peroxide usually have poor storage stability, which leads to various problems such as reduced hydrogen peroxide content, unstable effect, leakage of contents, and short shelf life. Summary of the Invention

[0004] Based on this, the purpose of this invention is to provide a teeth whitening composition with good storage stability and its preparation method, using a stabilizer combination scheme with small molecule organic amines having steric hindrance effect as the core, which significantly improves the storage stability of teeth whitening products containing peroxides.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a teeth whitening composition with good storage stability, comprising the following components by mass percentage: 60-70% hydrogen peroxide solution, 0.1-10% small molecule organic amine, 0.1-5% nonionic surfactant, 1-10% stabilizer, 4-6% thickener, 0.1-0.2% fragrance, 10-15% glycerol, and the balance being water, wherein the concentration of hydrogen peroxide is 30-50%; the small molecule organic amine compound is one of triethanolamine, trimethylamine, triethylamine, N-methyldiethanolamine, N-methyldicyclohexylamine, and N,N-diisopropylethylamine.

[0006] Preferably, the nonionic surfactant is one of fatty alcohol polyoxyethylene ethers, fatty acid polyoxyethylene esters, sorbitan fatty acid esters, or polyoxyethylene sorbitan fatty acid esters.

[0007] Preferably, the stabilizer is one or more of citric acid, disodium edetate, and hydroxyethylidene diphosphonic acid.

[0008] Preferably, the thickener is a copolymer of hydroxyethyl acrylate and sodium acryloyl dimethyl taurate.

[0009] Preferably, 0.1-0.5% of amorphous calcium fluorophosphate (ACFPC) is also added.

[0010] A method for preparing a teeth whitening composition with good storage stability is as follows: S1: Dissolve hydrogen peroxide solution, stabilizer, water, glycerol and small molecule organic amine by stirring to obtain a mixed solution; S2: Add flavoring and thickener to the mixed solution obtained in S1, and stir at a high speed of 1000~2000 rpm for 5 minutes; S3: Based on S2, add nonionic surfactant dropwise while stirring until the addition is complete, then stir at a high speed of 1000~2000 rpm for 5 minutes to obtain a gel-like substance; S4: The gel obtained in S3 is subjected to vacuum to remove the air mixed in during stirring, thus obtaining a teeth whitening composition with good storage stability.

[0011] A method for preparing a teeth whitening composition with good storage stability, wherein the preparation method with added ACFPC is as follows: S1: Dissolve hydrogen peroxide solution, stabilizer, water, glycerol and small molecule organic amine by stirring to obtain a mixed solution; S2: Add ACFPC to the mixed solution obtained in S1 and stir at 400~500 rpm for 5 minutes to obtain ACFPC dispersion sol; S3: Add fragrance and thickener to the ACFPC dispersion sol, and stir at a high speed of 1000~2000 rpm for 5 minutes; add AEO-9 dropwise while stirring until the addition is complete, and then stir at a high speed of 1000~2000 rpm for 5 minutes to obtain a gel-like substance; S4: The gel obtained in S3 is subjected to vacuum to remove the air mixed in during stirring, thus obtaining a teeth whitening composition with good storage stability.

[0012] The preferred amorphous calcium fluorophosphate conjugate (ACFPC) is prepared using the following steps: 1) Component A: Dissolve calcium chloride in water and filter out trace amounts of insoluble impurities to obtain component A; 2) Component B: Dissolve sodium pyrophosphate decahydrate, sodium dihydrogen phosphate dihydrate, anhydrous disodium hydrogen phosphate and sodium fluoride in water, and filter out trace amounts of insoluble impurities to obtain component B. 3) While stirring at 400~500 rpm, add component A to component B, filter the mixture, and then filter the primary filter cake obtained by vacuum filtration with an appropriate amount of anhydrous ethanol to disperse it and then filter it again to obtain the filter cake. 4) Place the filter cake obtained in the previous step in a 65℃ oven to dry. The dried material is then passed through a 200-mesh nylon sieve. The material that passes through the sieve is ACFPC.

[0013] The small-molecule organic amine compound in this invention contains an amino group, and the hydrogen atoms surrounding its nitrogen atom are replaced by other groups, thus forming a certain degree of steric hindrance. This invention uses triethanolamine, whose three ethoxy groups in its molecular structure form a physical barrier through steric repulsion, effectively blocking intermolecular collisions. Simultaneously, the nitrogen atom in this type of molecule's spatial configuration can capture free radicals and chelate free oxygen, thereby playing a stabilizing role for hydrogen peroxide molecules.

[0014] AEO-9, a nonionic surfactant derived from fatty alcohol polyoxyethylene ethers, has a synergistic effect when combined with small molecule organic amine compounds, further enhancing the stabilizing effect of hydrogen peroxide molecules in the stabilizer.

[0015] AE0-9, a nonionic surfactant, forms micelles in aqueous solution, encapsulating hydrogen peroxide molecules within a hydrophobic core or hydrophilic shell, reducing their contact with the external environment (metal ion impurities) and delaying decomposition. Simultaneously, the ether bonds (-O-) in its molecular structure can capture free radicals (such as ·OH) generated during hydrogen peroxide decomposition, blocking chain reactions and reducing hydrogen peroxide decomposition.

[0016] Triethanolamine and AEO-9, when combined with conventional hydrogen peroxide stabilizers such as citric acid, disodium edetate, and hydroxyethylidene diphosphonic acid, which are substances that chelate metal ion impurities, have a synergistic effect. The combination of triethanolamine and AEO-9 can further enhance the stabilizing effect on hydrogen peroxide molecules, significantly improving the storage stability of peroxide-containing teeth whitening products.

[0017] The ACFPC in this invention is an amorphous calcium fluorophosphate combination (ACFPC). This special type of combination is randomly composed of calcium ions, fluoride ions, and complex phosphate groups. When added in small amounts (e.g., about 0.3%), it forms an ACFPC dispersion sol (a thin, suspended sol) after being stirred and dispersed in the mixture. This dispersion can physically encapsulate and adsorb H2O2 molecules, reducing the probability of collisions between molecules and thus slowing down their spontaneous decomposition. It also isolates, to some extent, the influence of harmful impurities (such as metal ions) on the stability of H2O2. Simultaneously, the ACFPC dispersion sol can adsorb onto the container wall or the surface of any trace impurities, forming a passivation film that reduces the decomposition effect of these surfaces on H2O2, further improving the stability of the teeth whitening agent composition. When the ACFPC content increases to 0.5%, the ACFPC dispersion sol exhibits flocculation and stratification, and its stabilizing effect on H2O2 begins to weaken. Detailed Implementation

[0018] Example 1: A teeth whitening composition with good storage stability, comprising 60% of a 50% hydrogen peroxide solution, 10% glycerin, 1.5% triethanolamine, 1% citric acid, 1% disodium edetate, 0.1% of a 60% hydroxyethylidene diphosphonic acid, 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.5% AEO-9, 0.1% fragrance, and the balance being water.

[0019] A mixture of 1% citric acid, 1% disodium edetate, 60% of a 50% hydrogen peroxide solution, 0.1% of a 60% hydroxyethylidene diphosphonic acid, 21.8% water, 10% glycerol, and 1.5% triethanolamine was stirred and dissolved to obtain a mixed solution. 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer were added to the mixed solution, and the mixture was stirred at 1000-2000 rpm for 5 minutes. While stirring, 0.5% AEO-9 was added dropwise until the addition was complete, and the mixture was stirred at 1000-2000 rpm for another 5 minutes to obtain a gel-like substance. The air introduced during stirring was removed from the gel-like substance using a vacuum method, resulting in a teeth whitening composition with good storage stability.

[0020] Example 2: A teeth whitening composition with good storage stability, comprising 60% of a 50% hydrogen peroxide solution, 10% glycerin, 1.5% triethanolamine, 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.5% AEO-9, 0.1% fragrance, and the balance being water.

[0021] A 60% solution of 50% hydrogen peroxide, water, 10% glycerol, and 1.5% triethanolamine were dissolved by stirring to obtain a mixed solution. 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer were added to the mixed solution. The mixture was stirred at 1000-2000 rpm for 5 minutes. While stirring, 0.5% AEO-9 was added dropwise until the addition was complete. The mixture was then stirred at 1000-2000 rpm for another 5 minutes to obtain a gel-like substance. The air introduced during stirring was removed from the gel-like substance through vacuum, resulting in a teeth whitening composition with good storage stability.

[0022] Example 3: A teeth whitening composition with good storage stability, comprising 60% of a 50% hydrogen peroxide solution, 10% glycerin, 0% triethanolamine, 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.1% fragrance, and the balance being water.

[0023] A 60% solution of 50% hydrogen peroxide, water, and 10% glycerol were stirred to dissolve the mixture, resulting in a mixed solution. 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer were added to the mixed solution, and the mixture was stirred at 1000-2000 rpm for 10 minutes to obtain a gel. The air introduced during stirring was removed from the gel under vacuum, resulting in a teeth whitening composition with good storage stability.

[0024] Example 4: A teeth whitening composition with good storage stability, comprising 60% of a 50% hydrogen peroxide solution, 10% glycerin, 1.5% triethanolamine, 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.1% fragrance, 0.1% AEO-9, and the balance being water.

[0025] A 60% solution of 50% hydrogen peroxide, water, 10% glycerol, and 1.5% triethanolamine were dissolved by stirring to obtain a mixed solution. 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer were added to the mixed solution. The mixture was stirred at 1000-2000 rpm for 5 minutes. While stirring, 0.1% AEO-9 was added dropwise until the addition was complete. The mixture was then stirred at 1000-2000 rpm for another 5 minutes to obtain a gel-like substance. The air introduced during stirring was removed from the gel-like substance through vacuum, resulting in a teeth whitening composition with good storage stability.

[0026] Example 5: A teeth whitening composition with good storage stability, comprising 60% of a 50% hydrogen peroxide solution, 10% glycerin, 1.5% triethanolamine, 1% citric acid, 1% disodium edetate, 0.1% of a 60% hydroxyethylidene diphosphonic acid, 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.5% AEO-9, 0.3% ACFPC, 0.1% fragrance, and the balance being water.

[0027] A mixture of 1% citric acid, 1% disodium edetate, 60% of a 50% hydrogen peroxide solution, 0.1% of a 60% hydroxyethylidene diphosphonic acid, 21.5% water, 10% glycerol, and 1.5% triethanolamine was stirred and dissolved to obtain a mixed solution. 0.3% ACFPC was added to the mixed solution, and the mixture was stirred at 400-500 rpm for 5 minutes to obtain an ACFPC dispersion sol. 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer were added to the ACFPC dispersion sol, and the mixture was stirred at 1000-2000 rpm for 5 minutes. 0.5% AEO-9 was added dropwise while stirring until the addition was complete, and then the mixture was stirred at 1000-2000 rpm for another 5 minutes to obtain a gel. The obtained gel was then subjected to vacuum to remove air introduced during stirring, resulting in a teeth whitening composition with good storage stability.

[0028] The preparation steps for amorphous calcium fluorophosphate (ACFPC) are as follows: 1) Component A: Dissolve 144g of calcium chloride in 356g of water, and filter out trace amounts of insoluble impurities to obtain component A; 2) Component B: Dissolve 50g sodium pyrophosphate decahydrate, 150g sodium dihydrogen phosphate dihydrate, 50g anhydrous disodium hydrogen phosphate and 20g sodium fluoride in 1230g water, and filter out trace amounts of insoluble impurities to obtain component B. 3) While stirring at 400-500 rpm, add component A to component B, filter the mixture, and then filter the primary filter cake obtained by vacuum filtration with 500 ml of anhydrous ethanol to disperse it and then filter it again to obtain the filter cake. 4) Place the filter cake obtained in the previous step in a 65℃ oven to dry. The dried material is then passed through a 200-mesh nylon sieve. The material that passes through the sieve is ACFPC.

[0029] Comparative Example 1: A teeth whitening composition with good storage stability, as shown in Table 1. Table 1: Mass ratio of each component in Comparative Example 1

[0030] Comparative Example 2: A teeth whitening composition with good storage stability, as shown in Table 2. Table 2: Mass ratio of each component in Comparative Example 2

[0031] Comparative Example 3: A teeth whitening composition with good storage stability, as shown in Table 3. Table 3: Mass ratio of each component in Comparative Example 3

[0032] Comparative Example 4: A teeth whitening composition with good storage stability, as shown in Table 4. Table 4: Mass ratio of each component in Comparative Example 4

[0033] Comparative Example 5: A teeth whitening composition with good storage stability, as shown in Table 5. Table 5: Mass ratio of each component in Comparative Example 5

[0034] Comparative Example 6, a teeth whitening composition with good storage stability, as shown in Table 6. Table 6: Mass ratio of each component in Comparative Example 6

[0035] Comparative Example 7, a teeth whitening composition with good storage stability, as shown in Table 7. Table 7: Mass ratio of each component in Comparative Example 7

[0036] Comparative Example 8: A teeth whitening composition with good storage stability, as shown in Table 8. Table 8: Mass ratio of each component in Comparative Example 8 The preparation processes were the same in all comparative examples.

[0037] Stability test: The test method involves investigating hydrogen peroxide, a reactive strong oxidizing agent that readily decomposes into water and oxygen. During storage, hydrogen peroxide-containing teeth whitening products will continue to slowly decompose, generating oxygen. The accumulated pressure pushes the sealing stopper at the other end of the syringe until it bursts out, causing the gel contents to leak and the product to fail. This test uses accelerated aging at 37℃ for 4 weeks to test the change in stopper movement distance and hydrogen peroxide content, comparing the stability of different experimental groups. A smaller stopper movement distance and a less decrease in hydrogen peroxide content indicate better stability for that group of samples. The hydrogen peroxide content was determined according to the standard "YY / T0632-2008 Determination of Peroxide Content in Dental Bleaching Materials".

[0038] The gels obtained in each embodiment and comparative example were filled into plastic syringes for testing. The samples in each group were subjected to accelerated aging at 37℃ for 4 weeks. The changes in stopper movement distance and hydrogen peroxide content were tested to examine and compare the stability of each experimental group, as shown in Table 9. Table 9: Comparison Data of Hydrogen Peroxide Stability Experiments in Examples and Comparative Examples

[0039] As shown in Table 9, the addition of 1.5% triethanolamine and 0.5% AEO-9, combined with conventional hydrogen peroxide stabilizers, has a synergistic effect, which can further enhance the stabilization effect on hydrogen peroxide. After the sample was accelerated to 37°C for 4 weeks, the hydrogen peroxide content was still 29.2%, the hydrogen peroxide content decreased by only 0.8%, and the rubber stopper movement distance was only 7 mm.

[0040] Comparative Example 9: A teeth whitening composition with good storage stability, containing ACFPC as shown in Table 10. Table 10: Mass ratio of each component in Comparative Example 9

[0041] Comparative Example 10: A teeth whitening composition with good storage stability, containing ACFPC as shown in Table 11. Table 11: Mass ratio of each component in Comparative Example 10

[0042] The gels obtained in each of Examples 5, Comparative Examples 9, and Comparative Examples 10 were filled into plastic syringes for testing. The samples in each group were subjected to accelerated aging at 37℃ for 4 weeks. The changes in the displacement distance of the rubber stoppers and the hydrogen peroxide content were tested to examine and compare the stability of each experimental group, as shown in Table 12: Table 12: Comparison data of hydrogen peroxide stability experiments between Example 5 and Comparative Example 9 and Comparative Example 10

[0043] From Table 12, adding 0.3% ACFPC to the component results in the best stability of H2O2; combining Tables 12 and 9, it can be concluded that adding ACFPC to the component further improves the stability of H2O2.

Claims

1. A tooth whitening composition having good storage stability, characterized in that The composition comprises the following components in percentage of mass: 60-70% of hydrogen peroxide solution, 0.1-10% of small molecule organic amine, 0.1-5% of non-ionic surfactant, 1-10% of stabilizer, 4-6% of thickening agent, 0.1-0.2% of essence, 10-15% of glycerol, and the rest is water, wherein the concentration of the hydrogen peroxide solution is 30-50%; the small molecule organic amine compound is one of triethanolamine, trimethylamine, triethylamine, N-methyl diethanolamine, N-methyl dicyclohexylamine, and N,N-diisopropyl ethylamine.

2. A tooth whitening composition having good storage stability according to claim 1, characterized in that The non-ionic surfactant is one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, sorbitan fatty acid ester, and polyoxyethylene sorbitan fatty acid ester.

3. A tooth whitening composition having good storage stability according to claim 1, characterized in that The stabilizer is one or more of citric acid, disodium edetate, and hydroxyethylidene diphosphonic acid.

4. The tooth whitening composition with good storage stability according to claim 1, characterized in that The thickening agent is hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer.

5. The tooth whitening composition with good storage stability according to claim 1, characterized in that 0.1-0.5% of amorphous calcium fluoride phosphate compound ACFPC is further added.

6. A tooth whitening composition having good storage stability according to claim 5, wherein The amorphous calcium fluoride phosphate compound ACFPC is prepared by the following steps: 1) A component: calcium chloride is dissolved in water, and trace insoluble impurities are filtered to obtain the A component; 2) B component: sodium pyrophosphate decahydrate, sodium dihydrogen phosphate dihydrate, disodium hydrogen phosphate anhydrous, and sodium fluoride are dissolved in water, and trace insoluble impurities are filtered to obtain the B component; 3) Under the stirring state of 400-500 rpm, the A component is added to the B component, the mixed product is suction filtered, the primary filter cake obtained by suction filtration is dispersed by stirring with a proper amount of anhydrous ethanol, and then suction filtration is performed again to obtain a filter cake; 4) The filter cake obtained in the above step is placed in a 65°C oven for drying, and the dried material is sieved through a 200-mesh nylon screen, and the undersize material is the ACFPC.

7. A method for preparing a tooth whitening composition having good storage stability, using a tooth whitening composition having good storage stability according to any one of claims 1 to 4, characterized in that The preparation method is as follows: S1: hydrogen peroxide, stabilizer, water, glycerol, and small molecule organic amine are stirred and dissolved to obtain a mixed solution; S2: essence and thickening agent are added to the mixed solution obtained in S1, and high-speed stirring is performed at a stirring speed of 1000-2000 rpm for 5 minutes; S3: based on S2, non-ionic surfactant is added dropwise under stirring, and after the addition is completed, high-speed stirring is performed at a stirring speed of 1000-2000 rpm for 5 minutes to obtain a gel; S4: the gel obtained in S3 is subjected to vacuum to remove the air mixed in the stirring, and a tooth whitening composition with good storage stability is obtained.

8. A method for preparing a tooth whitening composition having good storage stability, using a tooth whitening composition having good storage stability according to any one of claims 1 to 5, characterized in that The preparation method is as follows: S1: hydrogen peroxide, stabilizer, water, glycerol, and small molecule organic amine are stirred and dissolved to obtain a mixed solution; S2: ACFPC is added to the mixed solution obtained in S1, and stirring is performed at a stirring speed of 400-500 rpm for 5 minutes to obtain an ACFPC dispersion sol; S3: essence and thickening agent are added to the ACFPC dispersion sol, and high-speed stirring is performed at a stirring speed of 1000-2000 rpm for 5 minutes; AEO-9 is added dropwise under stirring, and after the addition is completed, high-speed stirring is performed at a stirring speed of 1000-2000 rpm for 5 minutes to obtain a gel; S4: The gelatinous material obtained in S3 is degassed by stirring in air under vacuum to obtain a tooth whitening composition having good storage stability.

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