CN110652468A - Preparation method of tooth care material - Google Patents
Preparation method of tooth care material Download PDFInfo
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- CN110652468A CN110652468A CN201911064214.4A CN201911064214A CN110652468A CN 110652468 A CN110652468 A CN 110652468A CN 201911064214 A CN201911064214 A CN 201911064214A CN 110652468 A CN110652468 A CN 110652468A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/88—Polyamides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to a preparation method of a tooth care material, which is prepared by carrying polyaspartic acid sodium on porous hydroxyapatite powder. The powder prepared by the technology is safe and sanitary, can be used independently, and can also be used as an additive to be matched with toothpaste and mouthwash, wherein the hydroxyapatite has the effect of cleaning and repairing the surface of teeth, and the polyaspartic acid has the effect of inhibiting tooth stains and tartar.
Description
Technical Field
The invention relates to a preparation method of dental care materials, in particular to a preparation method based on hydroxyapatite and polyaspartic acid as basic raw materials.
Background
Hydroxyapatite (HA) is the main inorganic mineral component of human and animal bones, is non-toxic and non-irritating, can be directly integrated with bone tissue, and induces regeneration of bone and other tissues. Hydroxyapatite powder has good biocompatibility and bioactivity, is widely applied to repair and replacement technology of bones and tissues, has very wide application prospect in the field of biomedicine, and mature products entering the market at present comprise hydroxyapatite coatings of artificial joints, bioactive bone cement and the like.
Polyaspartic Acid (PASP) is a high molecular polymer formed by condensation polymerization of L-aspartic acid, and experiments show that sodium polyaspartate can be used for reducing the formation of tartar, effectively controlling the development of dental plaque and culturing a bacterial biofilm outside teeth. Meanwhile, the cleaning of stains and artificial pigments on teeth is increased, and the staining of teeth is reduced. However, due to the lack of suitable carriers, there is no application of polyaspartic acid for dental care on the market.
Disclosure of Invention
The invention aims to provide a safe and sanitary tooth care material, hydroxyapatite has the efficacy of cleaning and repairing the surface of teeth, and polyaspartic acid has the effect of inhibiting dental stains and tartar.
The invention relates to a preparation method of a tooth care material, which comprises the following steps of:
step 1, preparing a reaction solution, comprising: (NH4)2HP04 solution, template agent, foaming agent, nitric acid solution and calcium nitrate solution;
step 2, placing the (NH4)2HP04 solution into a hydrothermal reaction container, adding a template agent under the stirring condition, continuing to add a calcium nitrate solution and a foaming agent under the stirring condition after the (NH4)2HP04 solution and the template agent are uniformly mixed, adjusting the pH value by using a nitric acid solution, then placing the hydrothermal reaction container containing the reaction liquid into a reaction kettle, gradually heating to 180 ℃ in a muffle furnace, reacting for 5 hours at the temperature of 180 ℃, and naturally cooling;
step 3, centrifuging the mixture obtained in the step to remove supernatant, washing solids with distilled water, centrifuging to remove supernatant, circulating for 3 times, drying the remaining solids after removing the supernatant in an air environment of 50 ℃, and then putting the solids in a crucible and placing the crucible in a tubular furnace for calcination;
step 4, controlling the solid to be treated for 2 hours in the air environment at the temperature of not higher than 200 ℃ at the temperature rising speed of 5 ℃/min;
step 5, controlling the temperature rise speed of 5 ℃/min, treating the solid in an oxygen environment of 500-560 ℃, and naturally cooling to room temperature to obtain solid powder, namely porous hydroxyapatite powder;
and 6, putting the sintered powder into a solution of the sodium polyaspartate, stirring at the rotating speed of 60-150rpm for 1 hour, taking out, and drying at 60 ℃.
Further, the concentration of the (NH4)2HP04 solution is 0.05-0.1mol/L, the template agent is water-soluble starch, modified cellulose, soluble polysaccharide or a composition thereof, the concentration of the template agent is 0.1-0.5 wt% solution, the concentration of the nitric acid solution is 1.0-2.0mol/L, the concentration of the calcium nitrate solution is 0.01-0.05g/mL, the foaming agent is 0.01 wt% NaHCO3 or KHCO3, and the volume ratio of the (NH4)2HP04 is 1:18-1: 22.
Further, the volume ratio of the template agent to the (NH4)2HP04 solution is 1:0.9-1:1.1, and the pH of the reaction solution after adding nitric acid is 4.9-5.3, and the volume ratio of the (NH4)2HP04 solution to the calcium nitrate solution is 100:140-100: 180.
Further, the concentration of the sodium polyaspartate is 0.1 to 0.5 wt%.
The powder prepared by the technology is safe and sanitary, can be used independently, and can also be used as an additive component to be matched with toothpaste and mouthwash for use, wherein the hydroxyapatite has the effect of cleaning and repairing the surface of teeth, and the polyaspartic acid has the effect of inhibiting tooth stains and tartar.
Detailed Description
The technical scheme of the invention is as follows:
the invention relates to a preparation method of a tooth care material, which comprises the following steps of:
step 1, preparing a reaction solution, comprising: (NH4)2HP04 solution, template agent, foaming agent, nitric acid solution and calcium nitrate solution;
step 2, placing the (NH4)2HP04 solution into a hydrothermal reaction container, adding a template agent under the stirring condition, continuing to add a calcium nitrate solution and a foaming agent under the stirring condition after the (NH4)2HP04 solution and the template agent are uniformly mixed, adjusting the pH value by using a nitric acid solution, then placing the hydrothermal reaction container containing the reaction liquid into a reaction kettle, gradually heating to 180 ℃ in a muffle furnace, reacting for 5 hours at the temperature of 180 ℃, and naturally cooling;
step 3, centrifuging the mixture obtained in the step to remove supernatant, washing solids with distilled water, centrifuging to remove supernatant, circulating for 3 times, drying the remaining solids after removing the supernatant in an air environment of 50 ℃, and then putting the solids in a crucible and placing the crucible in a tubular furnace for calcination;
step 4, controlling the solid to be treated for 2 hours in the air environment at the temperature of not higher than 200 ℃ at the temperature rising speed of 5 ℃/min;
step 5, controlling the temperature rise speed of 5 ℃/min, treating the solid in an oxygen environment of 500-560 ℃, and naturally cooling to room temperature to obtain solid powder, namely porous hydroxyapatite powder;
and 6, putting the sintered powder into a solution of the sodium polyaspartate, stirring at the rotating speed of 60-150rpm for 1 hour, taking out, and drying at 60 ℃.
Further, the concentration of the (NH4)2HP04 solution is 0.05-0.1mol/L, the template agent is water-soluble starch, modified cellulose, soluble polysaccharide or a composition thereof, the concentration of the template agent is 0.1-0.5 wt% solution, the concentration of the nitric acid solution is 1.0-2.0mol/L, the concentration of the calcium nitrate solution is 0.01-0.05g/mL, the foaming agent is 0.01 wt% NaHCO3 or KHCO3, and the volume ratio of the (NH4)2HP04 is 1:18-1: 22.
Further, the volume ratio of the template agent to the (NH4)2HP04 solution is 1:0.9-1:1.1, and the pH of the reaction solution after adding nitric acid is 4.9-5.3, and the volume ratio of the (NH4)2HP04 solution to the calcium nitrate solution is 100:140-100: 180.
Further, the concentration of the sodium polyaspartate is 0.1 to 0.5 wt%.
Step 1 (NH4)2HP04, water-soluble starch, NaHCO3, nitric acid and calcium nitrate solution are prepared. Step 2, putting the (NH4)2HP04 solution into a hydrothermal reaction container, adding water-soluble starch under stirring, adding a calcium nitrate solution and NaHCO3 under stirring after uniformly mixing, and adjusting the pH value to 5.1 by using a nitric acid solution. Then placing the hydrothermal reaction container containing the reaction liquid into a reaction kettle, gradually raising the temperature to 180 ℃ in a muffle furnace, keeping the temperature at 180 ℃ for reaction for 5 hours, and then naturally cooling.
And 3, centrifuging the mixture reacted in the step 2 to remove supernatant, washing solids with distilled water, centrifuging to remove supernatant, circulating for 3 times, drying the remaining solids after the supernatant is removed in an air environment of 50 ℃, putting the dried solids in a crucible, and calcining in a tubular furnace, wherein the heating reaction process comprises the following three steps:
A. controlling the temperature rise speed of 5 ℃/min, and treating the solid in an air environment at the temperature of not higher than 200 ℃ for 2 h;
B. controlling the temperature rise speed of 5 ℃/min, and treating the solid in an oxygen environment at 500-560 ℃ for 3 h;
C. naturally cooling to room temperature to obtain solid powder, namely the porous hydroxyapatite powder.
And 4, putting the sintered powder into a solution of the sodium polyaspartate, stirring at the rotating speed of 120rpm for 1 hour, taking out, and drying at 60 ℃.
The specific embodiment is as follows: the parameters of the porous body obtained by different raw material ratios are as follows
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention relates, several simple deductions or substitutions may be made without departing from the spirit of the invention, and all shall be considered as belonging to the scope of the invention.
Claims (4)
1. A method for preparing a tooth care material, which is characterized by comprising the following steps: the preparation method of the porous hydroxyapatite powder and the polyaspartic acid sodium comprises the following steps:
step 1, preparing a reaction solution, comprising: (NH4)2HP04 solution, template agent, foaming agent, nitric acid solution and calcium nitrate solution;
step 2, placing the (NH4)2HP04 solution into a hydrothermal reaction container, adding a template agent under the stirring condition, continuing to add a calcium nitrate solution and a foaming agent under the stirring condition after the (NH4)2HP04 solution and the template agent are uniformly mixed, adjusting the pH value by using a nitric acid solution, then placing the hydrothermal reaction container containing the reaction liquid into a reaction kettle, gradually heating to 180 ℃ in a muffle furnace, reacting for 5 hours at the temperature of 180 ℃, and naturally cooling;
step 3, centrifuging the mixture obtained in the step to remove supernatant, washing solids with distilled water, centrifuging to remove supernatant, circulating for 3 times, drying the remaining solids after removing the supernatant in an air environment of 50 ℃, and then putting the solids in a crucible and placing the crucible in a tubular furnace for calcination;
step 4, controlling the solid to be treated for 2 hours in the air environment at the temperature of not higher than 200 ℃ at the temperature rising speed of 5 ℃/min;
step 5, controlling the temperature rise speed of 5 ℃/min, treating the solid in an oxygen environment of 500-560 ℃, and naturally cooling to room temperature to obtain solid powder, namely porous hydroxyapatite powder;
and 6, putting the sintered powder into a solution of the sodium polyaspartate, stirring at the rotating speed of 60-150rpm for 1 hour, taking out, and drying at 60 ℃.
2. The method for preparing a dental care material according to claim 1, characterized in that: the concentration of the (NH4)2HP04 solution is 0.05-0.1mol/L, the template agent is water-soluble starch, modified cellulose, soluble polysaccharide or a composition thereof, the concentration of the template agent is 0.1-0.5 wt% solution, the concentration of the nitric acid solution is 1.0-2.0mol/L, the concentration of the calcium nitrate solution is 0.01-0.05g/mL, the foaming agent is 0.01 wt% NaHCO3 or KHCO3, and the volume ratio of the (NH4)2HP04 is 1:18-1: 22.
3. The method for preparing a dental care material according to claim 1, characterized in that: the volume ratio of the template agent to the (NH4)2HP04 solution is 1:0.9-1:1.1, the pH of the reaction solution after adding nitric acid is 4.9-5.3, and the volume ratio of the (NH4)2HP04 solution to the calcium nitrate solution is 100:140-100: 180.
4. The method for preparing a dental care material according to claim 1, characterized in that: the concentration of the polyaspartic acid sodium is 0.1-0.5 wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911064214.4A CN110652468A (en) | 2019-11-04 | 2019-11-04 | Preparation method of tooth care material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911064214.4A CN110652468A (en) | 2019-11-04 | 2019-11-04 | Preparation method of tooth care material |
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| CN110652468A true CN110652468A (en) | 2020-01-07 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060280694A1 (en) * | 2005-06-09 | 2006-12-14 | John Peldyak | Composition for the mineralization of dental hard tissues and the reduction of caries-inducive microflora |
| CN108439360A (en) * | 2018-03-26 | 2018-08-24 | 广东药科大学附属第医院 | A kind of preparation method of spherical porous nanometer hydroxyapatite |
| CN109431860A (en) * | 2018-12-28 | 2019-03-08 | 北京焉支山科技有限公司 | Cosmetics-stage poly (sodium aspartate) and daily chemical product containing the ingredient |
-
2019
- 2019-11-04 CN CN201911064214.4A patent/CN110652468A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060280694A1 (en) * | 2005-06-09 | 2006-12-14 | John Peldyak | Composition for the mineralization of dental hard tissues and the reduction of caries-inducive microflora |
| CN108439360A (en) * | 2018-03-26 | 2018-08-24 | 广东药科大学附属第医院 | A kind of preparation method of spherical porous nanometer hydroxyapatite |
| CN109431860A (en) * | 2018-12-28 | 2019-03-08 | 北京焉支山科技有限公司 | Cosmetics-stage poly (sodium aspartate) and daily chemical product containing the ingredient |
Non-Patent Citations (1)
| Title |
|---|
| 裴立宅等: "《高技术陶瓷材料》", 31 July 2015, 合肥工业大学出版社 * |
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