CN1582888A - Nano toothpaste additive and its preparation - Google Patents
Nano toothpaste additive and its preparation Download PDFInfo
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- CN1582888A CN1582888A CN 200410046143 CN200410046143A CN1582888A CN 1582888 A CN1582888 A CN 1582888A CN 200410046143 CN200410046143 CN 200410046143 CN 200410046143 A CN200410046143 A CN 200410046143A CN 1582888 A CN1582888 A CN 1582888A
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Abstract
A nano-class additive for toothpaste is the strontium hydroxy phosphate: Ca10-xSrx(PO4)6(OH)2, where x=0-10. Its advantage are high desensitizing function, activity, and biocompatibility, no damage to tooth.
Description
Technical Field
The invention relates to a novel nano toothpaste additive and a synthesis method thereof, in particular to nano Ca10-xSrx(PO4)6(OH)2Wherein x is more than or equal to 0 and less than or equal to 10, belonging to the field of fine chemical engineering.
Background
The toothpaste usually contains abrasive, humectant, foaming agent, thickener, preservative, flavor enhancer, water, etc., and according to different uses, colorant, corrosion inhibitor, anticaries agent, antiplaque agent, anticalculus agent, anti-inflammatory agent, deodorant, desensitizer, etc. may be added. Wherein the desensitizing agent reduces dentinal hypersensitivity. Within the dentin are numerous dentinal tubules, which normally should be protected by the enamel or gums. When damaged enamel or gingival atrophy occurs, these tubules are in an externally "open" state, causing soreness when stimulated by external temperature (cold, heat), chemicals (sour, sweet), and mechanical action (abrasion or hard bite), resulting in tooth sensitivity. The dental caries can be avoided, the dentin tubules are blocked, the permeability of the hard tissues of the tooth body is reduced, the buffer effect of the tissues of the tooth body is improved, and the like, so that the dentin hypersensitivity can be effectively prevented. The desensitizer commonly used in toothpaste is strontium chloride, potassium nitrate, urea, Chinese herbal medicines, strontium hydroxyphosphate and the like, wherein the strontium chloride is widely applied. Chinese patent 1286623 discloses a desensitizing composition for teeth, which is prepared from soluble potassium salt and strontium salt as desensitizing agent, wherein strontium chloride is strontium salt. The Chinese patent 1305802 provides an oral desensitizing paste, which uses 5-15% of high-content strontium chloride, so that the desensitizing effect is more obvious. The nano strontium hydroxyphosphate developed by the method has better biocompatibility and the function of preventing decayed teeth, and the desensitizing and analgesic effects of the nano strontium hydroxyphosphate are obviously better than those of strontium chloride.
Disclosure of Invention
The invention aims to provide a novel nano toothpaste additive and a synthesis method thereof, in particular to nano Ca10-xSrx(PO4)6(OH)2Wherein x is more than or equal to 0 and less than or equal to 10, overcomes the defects of the toothpaste additive, and has the effects of preventing decayed teeth, preventing and treating tooth desensitization and directly repairing tooth abrasion.
The invention is based on the following principle: hydroxyapatite, Ca10(PO4)6(OH)2Is inorganic component forming hard tissue of vertebrates and human bodies, such as hydroxyapatite with 65 percent of human bone components and hydroxyapatite with more than 95 percent of human tooth surfaces, is nontoxic, is known as medical bioceramic star, and is biological materialThe most important one is good biocompatibility and bioactivity to soft tissue and hard tissue. Therefore, from the biological point of view, hydroxyapatite is the most suitable substitute material for hard tissues of living bodies, and does not have side effects on human bodies. The nano hydroxyapatite crystal is easy to grow, and 95% of the components on the surface of the tooth enamel are hydroxyapatite, so that the tooth enamel can directly repair the surface damage and decayed tooth.
Ca in hydroxyapatite2+Quilt Sr2+After partial or complete substitution, strontium-apatite (strontium hydroxyphosphate), i.e. Ca, is formed10-xSrx(PO4)6(OH)2Wherein x is more than or equal to 0 and less than or equal to 10. It has better biocompatibility than hydroxyapatite, can play a role in preventing decayed teeth, and can provide desensitization and analgesia functions.
The novel nanoscale toothpaste additive provided by the invention has the advantages that the particle size of the additive is nanoscale, and the particle size of the additive is preferably 10 +/-5-1000 +/-5 nm;
the additive is preferably Ca10-xSrx(PO4)6(OH)2Wherein x is more than or equal to 0 and less than or equal to 10, and can be added into various toothpastes with different efficacies;
the content of the additive in the toothpaste is 0.001-10% by weight.
The invention also provides a preparation method of the novel nano toothpaste additive, which comprises a physical method and a chemical method.
Physical methods such as mechanical pulverization methods including ball milling, vibratory milling, stirred milling, colloid milling, nano jet milling, and the like; the evaporation and condensation method includes a soot particle crystallization method, a vacuum evaporation deposition method on a flowing oil surface, a plasma heating method, a laser heating evaporation method, an electron beam heating evaporation method, an arc discharge heating evaporation method, a high-frequency induction heating evaporation method, a solar furnace heating evaporation method, and the like; an ion sputtering method; freeze drying; a spark discharge method; explosion sintering method. Chemical methods such as gas phase chemical reaction methods including gas phase decomposition method, gas phase synthesis method, gas-solid reaction method; the precipitation method comprises a coprecipitation method, a hydrolysis precipitation method and a hydrothermal synthesis method; spray pyrolysis method; solvent volatilization decomposition method; sol-gel method; electrochemical synthesis; radiation chemical synthesis method.
The nano additive of the present invention is synthesized by a sol-gel method, but the additive applied to the toothpaste is by no means limited by the synthesis method. The reaction formula is as follows:
wherein PO4 3-From H3PO4、K3PO4、Na3PO4、(NH4)3PO4、K2HPO4、Na2HPO4、(NH4)2HPO4Etc.; sr2+From Sr (OH)2、SrCl2、Sr(NO3)2Etc.; ca2+From CaO, Ca (OH)2、Ca(NO3)2、CaCl2Etc. OH-From Sr (OH)2、Ca(OH)2NaOH, KOH, etc.
The method comprises the following specific steps:
weighing a certain amount of Ca salt and Sr salt, preferably Sr (OH)2Adding CaO into a certain amount of deionized water, heating to 20-100 ℃ under the condition of stirring, preferably 60-80 ℃, and keeping the temperature to obtain an emulsion;
weighing a certain amount of phosphate according to the molar ratio of (Ca + Sr)/P of 1.67, dissolving the phosphate in a certain amount of deionized water, and slowly dropwise adding the phosphate into the mixed emulsion of Ca salt and Sr salt under the condition of constant-temperature stirring; after the dropwise addition is finished, dilute NaOH solution or dilute H is added3PO4Adjusting the pH value of the solution to about 7, keeping the temperature at 20-100 ℃, and preferably continuously stirring for 2 hours at 60-80 ℃;
stopping stirring, standing, and aging at room temperature for 0-10 days, preferably 4-6 days; filtering and drying to obtain white strontium apatite.
The novel nano toothpaste additive has the advantages that the novel nano toothpaste additive comprises the following aspects:
1. the additive is strontium hydroxyphosphate which has good desensitizing effect;
2. the additive has better biocompatibility than hydroxyapatite and can play a role in preventing decayed teeth; the additive has a structure similar to enamel on the surface of the tooth, has good biocompatibility and has no damage to the tooth and oral tissues;
3. the particle size of the additive is in a nanometer scale, the biological effect of the additive is enhanced by the nanometer size effect, the biological effect of the additive is favorably exerted, the activity is high, the additive is easy to adsorb on the surface of teeth or the abraded part to grow, and the killing power to bacteria is enhanced;
4. the nanometer additive particles also increase the lubricity of the toothpaste, and reduce the damage of the traditional toothpaste to the gum due to the friction of large particles;
5. the nano-scale additive also has whitening effect;
6. the toothpaste prepared by the nano-scale additive meets the national medical and health standards, does not produce side effects on human bodies, and is environment-friendly, thus being an ideal novel toothpaste additive.
Drawings
The attached figure I is as follows: sr synthesized from example 110(PO4)6(OH)2According to the Sherle formula, d is 0.89 lambda/(β cos theta), the grain size of the obtained sample is 22.6nm, and the numbers noted in the figure are the parameters of each main crystal face of the strontium apatite.
Detailed Description
Example 1
Weighing 10mmol Sr (OH)2·8H2Dissolving O in 60ml of water, stirring, heating to 80 ℃, and keeping the temperature constant; take 6mmol H3PO4Dissolving in 60ml water, stirring, and adding into Sr (OH) dropwise under stirring at constant temperature of 80 deg.C2·8H2O solutionIn the liquid. Adjusting pH to 7 after the dropwise addition, continuously stirring for 2h, stopping stirring, standing, aging for 5 days, vacuum filtering, and drying at 80 deg.C for 12h to obtain Sr10(PO4)6(OH)2。
Example 2
0.18mol of CaO and 0.02mol of SrCl are weighed2Slowly adding 120ml of water into a beaker, stirring, heating to 60 ℃, and keeping the temperature constant; simultaneously taking 0.12mol of H3PO4Stirring uniformly in a beaker containing 80ml of deionized water, transferring the mixture to a separating funnel, and gradually dropwise adding CaO and SrCl under the condition of stirring at constant temperature of 60 DEG C2In the mixed solution of (1). Adjusting pH to 7 after the dropwise addition, continuously stirring at constant temperature for 2h, stopping stirring, standing, aging for 5 days, filtering, washing, and drying at 80 deg.C for 12h to obtain Ca9Sr(PO4)6(OH)2。
Example 3
0.25mol CaO and 0.25mol Sr (OH) are weighed2·8H2Adding 300ml of water slowly into a beaker, stirring, heating to 60 ℃, and keeping the temperature constant; simultaneously taking 0.30mol of H3PO4Stirring uniformlyin a beaker containing 200ml of deionized water, transferring the mixture to a separating funnel, and gradually dropwise adding CaO, Sr and (OH) under the condition of stirring at the constant temperature of 60 DEG C2·8H2And O in the mixed solution. Adjusting pH to 7 after the dropwise addition, continuously stirring at constant temperature for 2h, stopping stirring, standing, aging for 5 days, filtering, and drying at 80 deg.C for 12h to obtain Ca5Sr5(PO4)6(OH)2。
Example 4
0.01g of Ca with a particle size of 10 +/-5 nm9.5Sr0.5(PO4)6(OH)249g of calcium hydrophosphate, 3g of sodium lauryl sulfate, 1.2g of carboxymethyl cellulose, 1g of sodium pyrophosphate, 0.3g of saccharin, 25g of glycerol, 1.3g of spice and deionized water are added to the total amount of 100g, and the toothpaste is prepared according to the common process of toothpaste production.
Example 5
0.5g of Ca with a particle size of 100 +/-5 nm9.5Sr0.5(PO4)6(OH)2Calcium hydrogen phosphate 75g, hydrolysis protease0.3g, 3g of surfactant, 0.5g of salt containing metal ions, 5g of adhesive, 0.05g of neutral protease,deionized water is added to total amount of 100g, and made into toothpaste according to conventional process for toothpaste production.
Example 6
10g of Ca with a particle size of 1000. + -.5 nm9.5Sr0.5(PO4)6(OH)250g of calcium hydrophosphate, 0.35g of saccharin, 20g of glycerol, 1.3g of spice, 2.5g of sodium lauryl sulfate, 1g of carboxymethyl cellulose, 0.5g of Chinese herbal medicine desensitizer, 0.5g of sodium pyrophosphate and deionized water, wherein the deionized water isadded to the total amount of 100g, and the toothpaste is prepared according to the common process of toothpaste production.
Example 7
0.01g of Ca with a particle size of 10 +/-5 nm9Sr(PO4)6(OH)20.4g of lauryl alcohol sulfate, 0.25g of sorbitol, 0.75g of monoglyceride lauryl sulfate, 1g of propylene glycol, 1.15g of carboxymethyl cellulose, 0.12g of saccharin, 39g of calcium pyrophosphate, 0.85g of spice, 0.4g of magnesium aluminosilicate, 18g of glycerol and deionized water are added to the total amount of 100g, and the toothpaste is prepared according to the common process of toothpaste production.
Example 8
0.5g of Ca with a particle size of 100 +/-5 nm9Sr(PO4)6(OH)251.7g of calcite, 0.3g of saccharin, 0.3g of calcium hydrophosphate, 1g of spice, 17g of glycerol, 0.04g of chlorophyll, 1.35g of carboxymethyl cellulose, 2.5g of sodium lauryl sulfate and deionized water, wherein the total amount is 100g, and the toothpaste is prepared according to the common process of toothpaste production.
Example 9
10g of Ca with a particle size of 1000. + -.5 nm9Sr(PO4)6(OH)215g of glycerol, 54g of natural calcium carbonate, 0.9g of carboxymethyl cellulose, 2.5g of sodium lauryl sulfate, 0.7g of hydroxyethyl cellulose, 0.35g of traditional Chinese medicine extract, 0.35g of saccharin, 1.1g of essence and deionized water are added to the total amount of 100g, and the toothpaste is prepared according to the common process of toothpaste production.
Example 10
0.01g of Sr with the grain diameter of 10 +/-5 nm10(PO4)(OH)218g of precipitated silicon dioxide, 15402.0 g ofpolyethylene glycol, 65.67g of 70% sorbitol, 1.5g of sodium lauryl sulfate, 0.7g of carboxymethyl cellulose, 1.25g of spice, 0.2g of saccharin, 1.8g of chloroform, 0.88g of color-imparting agent of 4% solution and deionized water are added to the total amount of 100g, and the toothpaste is prepared according to the common process of toothpaste production.
Example 11
0.1g of Sr with the grain diameter of 100 +/-5 nm10(PO4)(OH)20.3g of aluminum sulfate, 0.5g of sodium benzoate, 0.5g of 0.3-1.5 mm colored particles, 0.2g of saccharin, 22g of glycerol, 1.5g of sodium lauryl sulfate, 1g of carboxymethyl cellulose, 46.75g of calcium hydrophosphate dihydrate, 0.9g of spice and deionized water, wherein the total amount of the deionized water is 100g, and the toothpaste is prepared according to the common technology of toothpaste production.
Example 12
1.0g of Sr with the grain diameter of 1000 +/-5 nm10(PO4)(OH)250 parts of aluminum hydroxide, 1.3 parts of spice, 1.2 parts of carboxymethyl cellulose, 0.8 part of anticaries agent, 20 parts of glycerin, 0.2 part of corrosion inhibitor, 2.8 parts of surfactant, 0.35 part of saccharin and deionized water, wherein the total amount is 100 parts, and the toothpaste is prepared according to the common process of toothpaste production.
Claims (10)
1. A novel nano toothpaste additive is characterized in that the particle size is nano scale.
2. The nanoscale toothpaste additive according to claim 1, wherein the particle size of the additive is 10 ± 5 to 1000 ± 5 nm.
3. The nano-sized toothpaste additive according to claim 1 or 2, wherein the additive is Ca10-xSrx(PO4)6(OH)2Wherein x is more than or equal to 0 and less than or equal to 10.
4. The nanoscale toothpaste additive according to claim 1 or 2, wherein the content of the additive in the toothpaste is 0.01-10% by weight;
5. the method for preparing nano-sized toothpaste additive according to claim 3, wherein the Ca is10-xSrx(PO4)6(OH)2The additive may be synthesized in aqueous solution by a sol-gel method, but is in no way limited to what method is used to synthesize the additive.
6. The method for preparing nano-sized toothpaste additive according to claim 5, further comprising PO4 3-、Ca2+And Sr2+And OH in stoichiometric ratio in aqueous solution.
7. The method for preparing a nano-sized toothpaste additive according to claim 5, wherein the reaction temperature is 20 to 100 ℃, preferably 60 to 80 ℃.
8. The method for preparing a nano-sized toothpaste additive according to claim 5, wherein the reaction is carried out under stirring.
9. The method for preparing nano-sized toothpaste additive according to claim 6, wherein PO is4 3-From H3PO4、K3PO4、Na3PO4、(NH4)3PO4、K2HPO4、Na2HPO4、(NH4)2HPO4；Sr2+From Sr (OH)2、SrCl2、Sr(NO3)2；Ca2+From CaO, Ca (OH)2、Ca(NO3)2、CaCl2；OH-From Sr (OH)2、CaO、Ca(OH)2、NaOH、KOH。
10. The method of claim 6, wherein PO is4 3-The concentration is 0-3 mol/L; ca2+Sr at a concentration of 0 to 5mol/L2+The concentration is 0 to 5mol/L，OH-The concentration is 0 to 1 mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105534792A (en) * | 2015-12-16 | 2016-05-04 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Chinese herbal medicine toothpaste containing nano diamond olefine |
| CN105534725A (en) * | 2015-12-16 | 2016-05-04 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Comprehensive functional toothpaste containing nano diamond alkene |
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2004
- 2004-06-03 CN CN 200410046143 patent/CN1582888A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105534792A (en) * | 2015-12-16 | 2016-05-04 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Chinese herbal medicine toothpaste containing nano diamond olefine |
| CN105534725A (en) * | 2015-12-16 | 2016-05-04 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Comprehensive functional toothpaste containing nano diamond alkene |
| CN105534792B (en) * | 2015-12-16 | 2018-05-18 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of Chinese herbal toothpaste containing nanometer diamond alkene |
| CN105534725B (en) * | 2015-12-16 | 2018-05-18 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of comprehensive function type toothpaste containing nanometer diamond alkene |
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