阅读说明：本技术 一种牙齿护理材料制备方法 (Preparation method of tooth care material ) 是由 吴有庭 陈雷 庄薇娜 于 2019-11-04 设计创作，主要内容包括：本发明一种牙齿护理材料制备方法,是以多孔羟基磷灰石粉体搭载聚天冬氨酸钠制备得到。该技术制备的粉体安全卫生,可以单独使用,也可作为添加成分与牙膏、漱口水配合使用,其中的羟基磷灰石具有清洁和修护牙齿表面的功效,聚天冬氨酸则具有抑制牙渍和牙石的效果。(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.)

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%.

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 ℃.