A tooth whitening composition having good storage stability and a method of preparing the same

Abstract

The application discloses a tooth whitening composition with good storage stability and a preparation method thereof, and comprises 60-70% of a hydrogen peroxide solution, 0.1-10% of a small-molecule organic amine, 0.1-5% of a non-ionic surfactant, 1-10% of a stabilizer, 4-6% of a thickening agent, 0.1-0.2% of a fragrance, 10-15% of glycerol, and the balance of water. The hydrogen peroxide, the stabilizer, water, glycerol and the small-molecule organic amine are stirred and dissolved to obtain a mixed solution; the fragrance and the thickening agent are added into the mixed solution, and high-speed stirring is carried out at a stirring speed of 1000-2000 rpm for 5 minutes; the non-ionic surfactant is added dropwise in a stirring state, and after dropwise addition is completed, high-speed stirring is carried out at a stirring speed of 1000-2000 rpm for 5 minutes, so that a tooth whitening composition with good storage stability is obtained. The stabilizer combination scheme with the small-molecule organic amine as the core and with the space steric hindrance effect is used, and the storage stability of a peroxide-containing tooth whitening product is remarkably improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of tooth whitening compositions, in particular to a tooth whitening composition with good storage stability and a preparation method thereof. BACKGROUND

[0002] The main methods of tooth whitening are chemical bleaching by drugs, covering and whitening, etc., and also reducing the natural color of teeth by tooth cleaning, sand blasting and other methods. With the increasing development of cosmetic dentistry, the chemical bleaching method containing peroxide is becoming more and more popular. This method is through the oxidation-reduction chemical reaction of peroxide to decompose the organic dye macromolecules on the surface of teeth into small molecules, so that the color of the small molecules becomes lighter, the pigments on the surface and deep layer of teeth are lightened, and the teeth are whitened. The most commonly used effective chemical components for tooth whitening are hydrogen peroxide or urea peroxide, and the core effective component of urea peroxide is still hydrogen peroxide.

[0003] Hydrogen peroxide is a strong oxidizing agent, which is easy to decompose into water and oxygen. The tooth whitening products containing hydrogen peroxide will continuously decompose as soon as they are produced. If they are affected by various factors such as temperature, metal ion pollution, alkaline environment, light, etc., the decomposition reaction will be further intensified. Therefore, the tooth whitening products containing hydrogen peroxide usually have poor storage stability, which leads to various problems such as reduction of hydrogen peroxide content, unstable effect, content swelling and leakage, short shelf life, etc. SUMMARY

[0004] Therefore, the present application aims to provide a tooth whitening composition with good storage stability and a preparation method thereof. The stabilizer group scheme with small molecule organic amine as the core with steric hindrance effect significantly improves the storage stability of the tooth whitening products containing peroxide.

[0005] To achieve the above-mentioned purpose, the present application provides the following technical scheme: a tooth whitening composition with good storage stability, comprising the following components in mass percentage: 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 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-methyl diethanolamine, N-methyl dicyclohexylamine and N,N-diisopropyl ethylamine.

[0006] Preferably, 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.

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

[0008] Preferably, the thickening agent is hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer.

[0009] Preferably, 0.1-0.5% of amorphous calcium fluoride phosphate compound ACFPC is also added.

[0010] A method for preparing a tooth whitening composition with good storage stability, the preparation method is as follows:

[0011] S1: hydrogen peroxide solution, stabilizer, water, glycerol and small molecule organic amine are stirred and dissolved to obtain a mixed solution;

[0012] S2: add essence and thickening agent to the mixed solution obtained in S1, and stir at a speed of 1000-2000 rpm for 5 minutes;

[0013] S3: based on S2, add non-ionic surfactant dropwise under stirring, and then stir at a speed of 1000-2000 rpm for 5 minutes after the addition is completed, to obtain a gel;

[0014] S4: remove the air mixed by stirring from the gel obtained in S3 by vacuum, to obtain a tooth whitening composition with good storage stability.

[0015] A method for preparing a tooth whitening composition with good storage stability, the preparation method is as follows:

[0016] S1: hydrogen peroxide solution, stabilizer, water, glycerol and small molecule organic amine are stirred and dissolved to obtain a mixed solution;

[0017] S2: add ACFPC to the mixed solution obtained in S1, and stir at a speed of 400-500 rpm for 5 minutes to obtain an ACFPC dispersion sol;

[0018] S3: add essence and thickening agent to the ACFPC dispersion sol, and stir at a speed of 1000-2000 rpm for 5 minutes; add AEO-9 dropwise under stirring, and then stir at a speed of 1000-2000 rpm for 5 minutes after the addition is completed, to obtain a gel;

[0019] S4: remove the air mixed by stirring from the gel obtained in S3 by vacuum, to obtain a tooth whitening composition with good storage stability.

[0020] Preferably, the amorphous calcium fluoride phosphate compound ACFPC is prepared by the following steps:

[0021] 1), A component: dissolve calcium chloride in water, filter out trace insoluble impurities to obtain A component;

[0022] 2), B component: dissolve sodium pyrophosphate decahydrate, sodium dihydrogen phosphate dihydrate, disodium hydrogen phosphate anhydrous and sodium fluoride in water, filter out trace insoluble impurities to obtain B component;

[0023] 3), under the condition of stirring at a speed of 400-500 rpm, A component is added to B component, the mixed product is suction filtered, the primary filter cake obtained by suction filtration is dispersed by stirring with an appropriate amount of anhydrous ethanol and then suction filtered again to obtain a filter cake;

[0024] 4), the filter cake obtained in the above step is placed in a 65℃ oven for drying, and the dried material is sieved through a 200 mesh nylon screen, and the undersize is ACFPC.

[0025] The small-molecule organic amine compound in the application contains an amino group, the hydrogen atoms around the nitrogen atom of which are replaced by other groups, thereby forming a certain degree of steric hindrance effect. The application adopts triethanolamine, the three ethoxy groups in the molecular structure of which form a physical barrier through steric exclusion effect, which can effectively block the intermolecular collision, and the nitrogen atom of the spatial configuration of the molecule can capture free radicals to chelate free oxygen, thereby playing a stabilizing role on the hydrogen peroxide molecules.

[0026] The fatty alcohol polyoxyethylene ether nonionic surfactant AE0-9 has a synergistic effect when matched with the small-molecule organic amine compound, and can further improve the stabilizing effect of the stabilizer on the hydrogen peroxide molecules.

[0027] The AE0-9 nonionic surfactant forms micelles in an aqueous solution, wraps the hydrogen peroxide molecules in a hydrophobic core or a hydrophilic shell layer, reduces the contact of the hydrogen peroxide molecules with the external environment (metal ion impurities), and delays the decomposition. At the same time, the ether bond (-O-) in the molecular structure of the AE0-9 nonionic surfactant can capture free radicals (such as ·OH) generated by the decomposition of hydrogen peroxide, block the chain reaction, and reduce the decomposition of hydrogen peroxide:

[0028]

[0029] The triethanolamine and AE0-9 are matched with conventional hydrogen peroxide stabilizers, such as citric acid, disodium edetate, hydroxyethylidene diphosphonic acid and other substances that can chelate metal ion impurities, and have a synergistic effect. The combination of triethanolamine and AE0-9 can further improve the stabilizing effect on hydrogen peroxide molecules, and significantly improve the storage stability of peroxide-containing tooth whitening products.

[0030] The ACFPC in the present application is an amorphous calcium fluoro phosphate combination (ACFPC for short). The combination in this special form is randomly combined by calcium ions, fluorine ions and complex phosphate radicals. When a small amount (such as about 0.3%) is added and stirred and dispersed in a mixed solution, an ACFPC dispersion sol (a suspended thin sol form) can be formed. The ACFPC dispersion sol can physically wrap and adsorb H2O2 molecules, reduce the collision probability between the molecules, slow down the spontaneous decomposition of the molecules, and to some extent, isolate the influence of harmful impurities (such as metal ions) on the stability of H2O2. At the same time, the ACFPC dispersion sol can be adsorbed on the surface of the container wall or the trace impurities that may exist, forming a passivation film, reducing the decomposition of H2O2 by these surfaces, and further improving the stability of the tooth whitening agent composition. When the ACFPC addition amount is increased to 0.5%, the ACFPC dispersion sol will appear flocculation and stratification, and the stabilizing effect on H2O2 will begin to weaken. DETAILED DESCRIPTION

[0031] Example 1, a tooth whitening composition with good storage stability, comprising 60% of a hydrogen peroxide solution with a concentration of 50%, 10% glycerol, 1.5% triethanolamine, 1% citric acid, 1% disodium edetate, 0.1% hydroxyethylidene diphosphonic acid with a concentration of 60%, 4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.5% AEO-9, 0.1% fragrance, and the balance being water.

[0032] 1% citric acid, 1% disodium edetate, 60% of a hydrogen peroxide solution with a concentration of 50%, 0.1% hydroxyethylidene diphosphonic acid with a concentration of 60%, 21.8% water, 10% glycerol, and 1.5% triethanolamine are stirred and dissolved to obtain a mixed solution; 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer are added to the mixed solution, and stirred at a stirring speed of 1000-2000 rpm for 5 minutes; 0.5% AEO-9 is added dropwise under stirring, and after the dropwise addition is completed, the mixture is stirred at a stirring speed of 1000-2000 rpm for 5 minutes to obtain a gel; and the air mixed in the stirring is removed from the gel by vacuum to obtain a tooth whitening composition with good storage stability.

[0033] Example 2, a tooth whitening composition with good storage stability, comprising 60% of a hydrogen peroxide solution with a concentration of 50%, 10% glycerol, 1.5% triethanolamine, 4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.5% AEO-9, 0.1% fragrance, and the balance being water.

[0034] Dissolve 60% of 50% concentration hydrogen peroxide solution, water, 10% glycerin, 1.5% triethanolamine by stirring to obtain a mixed solution; add 0.1% essence, 4% hydroxyethyl acrylate / acryloyl dimethyl sodium taurate copolymer into the mixed solution, stir at 1000-2000 rpm for 5 minutes, drop 0.5% AEO-9 under stirring until the dropping is completed, then stir at 1000-2000 rpm for 5 minutes, obtain a gel; remove the air mixed by stirring from the obtained gel by vacuum, thus a tooth whitening composition with good storage stability is obtained.

[0035] Example 3, a tooth whitening composition with good storage stability, comprises 60% of 50% concentration hydrogen peroxide solution, 10% glycerin, 0% triethanolamine, 4% hydroxyethyl acrylate / acryloyl dimethyl sodium taurate copolymer, 0.1% essence, and the balance is water.

[0036] Dissolve 60% of 50% concentration hydrogen peroxide solution, water, 10% glycerin by stirring to obtain a mixed solution; add 0.1% essence, 4% hydroxyethyl acrylate / acryloyl dimethyl sodium taurate copolymer into the mixed solution, stir at 1000-2000 rpm for 10 minutes, obtain a gel; remove the air mixed by stirring from the obtained gel by vacuum, thus a tooth whitening composition with good storage stability is obtained.

[0037] Example 4, a tooth whitening composition with good storage stability, comprises 60% of 50% concentration hydrogen peroxide solution, 10% glycerin, 1.5% triethanolamine, 4% hydroxyethyl acrylate / acryloyl dimethyl sodium taurate copolymer, 0.1% essence, 0.1% AEO-9, and the balance is water.

[0038] Dissolve 60% of 50% concentration hydrogen peroxide solution, water, 10% glycerin, 1.5% triethanolamine by stirring to obtain a mixed solution; add 0.1% essence, 4% hydroxyethyl acrylate / acryloyl dimethyl sodium taurate copolymer into the mixed solution, stir at 1000-2000 rpm for 5 minutes, drop 0.1% AEO-9 under stirring until the dropping is completed, then stir at 1000-2000 rpm for 5 minutes, obtain a gel; remove the air mixed by stirring from the obtained gel by vacuum, thus a tooth whitening composition with good storage stability is obtained.

[0039] Example 5, a tooth whitening composition with good storage stability, comprising 60% of hydrogen peroxide solution with concentration of 50%, 10% glycerin, 1.5% triethanolamine, 1% citric acid, 1% disodium edetate, 0.1% hydroxyethylidene diphosphonic acid with concentration of 60%, 4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.5% AEO-9, 0.3% ACFPC, 0.1% fragrance, and the balance being water.

[0040] A mixture solution was prepared by stirring and dissolving 1% citric acid, 1% disodium edetate, 60% of hydrogen peroxide solution with concentration of 50%, 0.1% hydroxyethylidene diphosphonic acid with concentration of 60%, 21.5% water, 10% glycerin and 1.5% triethanolamine; 0.3% ACFPC was added into the mixture solution, and stirred at a stirring speed of 400-500 rpm for 5 minutes to obtain an ACFPC dispersion sol; 0.1% fragrance and 4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer were added into the ACFPC dispersion sol, and stirred at a stirring speed of 1000-2000 rpm for 5 minutes; 0.5% AEO-9 was added dropwise into the stirred mixture, and after the addition was completed, the mixture was stirred at a stirring speed of 1000-2000 rpm for 5 minutes to obtain a gel; the air mixed in the gel was removed by vacuum to obtain a tooth whitening composition with good storage stability.

[0041] The amorphous calcium fluoride phosphate compound ACFPC was prepared by the following steps:

[0042] 1) A component: 144 g of calcium chloride was dissolved in 356 g of water, and the trace insoluble impurities were filtered to obtain the A component;

[0043] 2) B component: 50 g of sodium pyrophosphate decahydrate, 150 g of sodium phosphate dibasic dihydrate, 50 g of sodium phosphate dibasic anhydrous and 20 g of sodium fluoride were dissolved in 1230 g of water, and the trace insoluble impurities were filtered to obtain the B component;

[0044] 3) The A component was added to the B component under stirring at a stirring speed of 400-500 rpm, and the mixed product was suction filtered; the primary filter cake obtained by suction filtration was dispersed by stirring in 500 ml of anhydrous ethanol, and then suction filtered again to obtain a filter cake;

[0045] 4) The filter cake obtained in the above step was placed in an oven at 65°C for drying, and the dried material was sieved through a 200 mesh nylon screen; the sieve residue was the ACFPC.

[0046] Comparative Example 1: a tooth whitening composition with good storage stability, as shown in Table 1,

[0047] Table 1: mass ratio of each component in Comparative Example 1

[0048] Comparative Example 1: a tooth whitening composition with good storage stability, as shown in Table 1,

[0049] Comparative Example 2: A tooth whitening composition with good storage stability, as shown in Table II,

[0050] Table II: Mass ratio of each component of Comparative Example 2

[0051]

[0052] Comparative Example 3: A tooth whitening composition with good storage stability, as shown in Table III,

[0053] Table III: Mass ratio of each component of Comparative Example 3

[0054]

[0055] Comparative Example 4: A tooth whitening composition with good storage stability, as shown in Table IV,

[0056] Table IV: Mass ratio of each component of Comparative Example 4

[0057]

[0058] Comparative Example 5: A tooth whitening composition with good storage stability, as shown in Table V,

[0059] Table V: Mass ratio of each component of Comparative Example 5

[0060]

[0061] Comparative Example 6: A tooth whitening composition with good storage stability, as shown in Table VI,

[0062] Table VI: Mass ratio of each component of Comparative Example 6

[0063]

[0064] Comparative Example 7: A tooth whitening composition with good storage stability, as shown in Table VII,

[0065] Table VII: Mass ratio of each component of Comparative Example 7

[0066]

[0067] Comparative Example 8: A tooth whitening composition with good storage stability, as shown in Table VIII,

[0068] Table VIII: Mass ratio of each component of Comparative Example 8

[0069]

[0070] The preparation process in each comparative example is the same.

[0071] Stability test:

[0072] Test method, hydrogen peroxide is a strong oxidizing agent, easy to decompose into water and oxygen, hydrogen peroxide containing tooth whitening products will continue to slowly decompose during storage to produce oxygen, the accumulated gas pressure pushes the sealing plug at the other end of the syringe to move until the plug collapses, the gel content is inflated, and the product is invalid. In this test, the stability of each experimental group was compared by testing the moving distance of the plug and the change of hydrogen peroxide content after 4 weeks of 37℃ accelerated aging. The smaller the moving distance of the plug, the less the hydrogen peroxide content decreases, indicating that the stability of the sample is better. The hydrogen peroxide content determination method is operated according to the standard of "YY / T0632-2008 Determination of Peroxide Content in Dental Bleaching Materials".

[0073] The gel obtained in each example and comparative example was filled into a plastic syringe, and the gel was filled into a plastic syringe;

[0074] Each group of samples was subjected to 37℃ accelerated aging for 4 weeks, and the moving distance of the plug and the change of hydrogen peroxide content were tested to compare the stability of each experimental group, as shown in Table Nine:

[0075] Table Nine: Comparison data of hydrogen peroxide stability experiment of examples and comparative examples

[0076]

[0077] From Table Nine, on the basis of adding 1.5% triethanolamine and 0.5% AEO-9, the conventional hydrogen peroxide stabilizer plays a synergistic role, which can further improve the stability of hydrogen peroxide. After 4 weeks of 37℃ accelerated aging, the hydrogen peroxide content is still 29.2%, the hydrogen peroxide content decreases by only 0.8%, and the moving distance of the plug is only 7mm.

[0078] Comparative Example 9: A tooth whitening composition with good storage stability, adding ACFPC as shown in Table Ten,

[0079] Table Ten: Mass ratio of each component of comparative example 9

[0080]

[0081] Comparative Example 10: A tooth whitening composition with good storage stability, adding ACFPC as shown in Table Eleven,

[0082] Table Eleven: Mass ratio of each component of comparative example 10

[0083]

[0084] The gelatinous substances obtained in Example 5 and Comparative Examples 9 and 10 were filled into plastic syringes and tested;

[0085] Each group of samples was subjected to accelerated aging at 37°C for 4 weeks, and the stability of each group was compared by testing the movement distance of the stopper and the change in the hydrogen peroxide content. The results are shown in Table 12:

[0086] Table 12: Comparison of hydrogen peroxide stability test data for Example 5 and Comparative Examples 9 and 10

[0087]

[0088] From Table 12, the addition of 0.3% ACFPC to the components resulted in the best H2O2 stability. In combination with Tables 12 and 9, it was concluded that the addition of ACFPC to the components resulted in better H2O2 stability.

Claims

1. A teeth whitening composition with good storage stability, characterized in that... It comprises 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, 0.1-0.3% amorphous calcium fluorophosphate (ACFPC), and the balance being water, wherein the concentration of hydrogen peroxide solution is 30-50%; the small molecule organic amine compound is one of triethanolamine, trimethylamine, triethylamine, N-methyldiethanolamine, N-methyldicyclohexylamine, and N,N-diisopropylethylamine; The amorphous calcium fluorophosphate conjugate ACFPC is prepared by 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.

2. The teeth whitening composition with good storage stability according to claim 1, characterized in that... The nonionic surfactant is one of the following: fatty alcohol polyoxyethylene ethers, fatty acid polyoxyethylene esters, sorbitan fatty acid esters, and polyoxyethylene sorbitan fatty acid esters.

3. The teeth whitening composition with 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 teeth whitening composition with good storage stability according to claim 1, characterized in that... The thickener is a copolymer of hydroxyethyl acrylate and sodium acryloyl dimethyl taurate.

5. A method for preparing a teeth whitening composition with good storage stability, comprising using a teeth whitening composition with good storage stability as described in any one of claims 1-4, characterized in that... The preparation method is as follows: S1: Dissolve hydrogen peroxide, 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.

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