CN102274127B - Tooth enamel caries prevention repair coating agent and use method thereof - Google Patents
Tooth enamel caries prevention repair coating agent and use method thereof Download PDFInfo
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- CN102274127B CN102274127B CN2011102035177A CN201110203517A CN102274127B CN 102274127 B CN102274127 B CN 102274127B CN 2011102035177 A CN2011102035177 A CN 2011102035177A CN 201110203517 A CN201110203517 A CN 201110203517A CN 102274127 B CN102274127 B CN 102274127B
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- tooth enamel
- enamel
- coating agent
- caries prevention
- tooth
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Abstract
The invention relates to a tooth repair coating agent, and particularly relates to a tooth enamel caries prevention repair coating agent and a use method thereof. The tooth enamel caries prevention repair coating agent can form a high-hardness high-wear-resistance coating layer capable of tightly combining with tooth enamel on the surface of the tooth enamel, so as to prevent and repair tooth enamel caries. The tooth enamel caries prevention repair coating agent comprises solid powder and cement liquid, wherein the solid powder is hydroxyapatite powder, and the cement liquid is at least one of phosphoric acid and hydrogen peroxide. The use method comprises the following steps: pretreating tooth enamel surface with a surface treatment agent, blending the solid powder and the cement liquid into the tooth enamel caries prevention repair coating agent, coating the tooth enamel caries prevention repair coating agent on the surface of a tooth sample, and cleaning away residual coating agent to complete tooth enamel caries prevention repair.
Description
Technical field
The present invention relates to a kind of tooth paint for repairing, especially relate to a kind of enamel preventing decayed tooth paint for repairing and method for using thereof.
Background technology
Dental caries be a kind of be pathogen with the antibacterial, multiple factor is participated in, occur in hard tooth tissue chronic, progressive destructive disease (height is learnt military affairs. clinical cariology [M]. medical science publishing house of Peking University, 2007).Dental caries and secondary disease thereof bring very big harm for human oral cavity even whole body health; Its sickness rate in the crowd is very high; World Health Organization (WHO) classifies it as one of three big diseases of harm humans; Its harm is of all ages, sex, ethnic group and area, each national resident all receive dental caries invasion and attack (Yue Songling. modern cariology [M]. combined publication society of China Concord Medical Science University of Beijing Medical University, 1993).
At present, the method for prevention and treatment dental caries mainly comprises 5 aspects: one is to use antibacterial that dental caries is prevented, and can obtain the effect of anti-dental caries really in a short time, but because life-time service can cause oral cavity flora imbalance, less at present application.The 2nd, utilize fluoride that dental caries is prevented and treated; This is to use preventing decayed tooth technology the most widely at present; Through the low concentration high-frequency fluorine of using, can effectively prevent dental caries generation (Fan Mingwen, Zhou Xuedong. endodontics [M]. the People's Health Publisher; 2008), but this method decrease for substantial dental caries and do not have good effect.The 3rd, the sealing of nest ditch, this technology is the generation of prophylaxis of teeth nest ditch place dental caries successfully, but can't prevent the dental caries at other positions to decrease, and along with the prolongation of service time has certain expulsion rate.Four are to use packing material, and this method can be decreased the position to dental caries effectively and filled, and stops further developing of dental caries, but need in the treatment to remove the healthy dental tissue of part, are not very ideal Therapeutic Method for enamel caries.
Hydroxyapatite is a kind of bioactive materials best with the body bone tissue biocompatibility of generally acknowledging at present; Biological hard tissue reparation and replacement field (Zheng Yufeng have been widely used in; Li Li. bio-medical material is learned [M]. publishing house of Harbin Institute of Technology, 2005).Because hydroxyapatite has identical inorganic constituents (Yang Shunqing with the tooth and the osseous tissue of human body; The hair tawny daylily. inorganic bio is learned [M]. the .2008 of publishing house of South China Science & Engineering University); Therefore it and enamel have closely similar thermal coefficient of expansion; The phenomenon that ftractures, come off in use can not occur, have incomparable advantage in the dental prosthetic field.
Summary of the invention
The present invention aim to provide a kind of can enamel surface form high rigidity, high-wearing feature, can with the enamel coating of combining closely, thereby reach the enamel preventing decayed tooth paint for repairing and the method for using thereof of prevention and repairing dental enamel dental caries damage.
Said enamel preventing decayed tooth paint for repairing comprises pressed powder and consolidation liquid, and said pressed powder is a hydroxyapatite powder, and said consolidation liquid is at least a in phosphoric acid, the hydrogen peroxide.
The calcium-phosphorus ratio of said hydroxyapatite powder can be 1.67, and the particle diameter of said hydroxyapatite powder can be 5～40 μ m, is good with 5～20 μ m.
Said consolidation liquid is preferably the mixed solution of phosphoric acid and hydrogen peroxide, and in the mixed solution of phosphoric acid and hydrogen peroxide, the volume ratio of phosphoric acid and hydrogen peroxide can be (0.1～0.5): 1; The mass percent concentration of said phosphoric acid can be 85%, and the mass percent concentration of said hydrogen peroxide can be 30%.
The method for using of said enamel preventing decayed tooth paint for repairing is following:
1) with surface conditioning agent enamel surface is carried out pretreatment;
In step 1), said surface conditioning agent is at least a in pickling agent and the alkali treatment liquid; Said pickling agent can be a kind of in phosphoric acid solution, citric acid solution or the lactic acid solution etc., the pH value of said pickling agent can≤3, be good with≤0.05, the said pretreated time can be 5～120s, is good with 20～40s; Said alkali treatment liquid can be sodium hydroxide solution or aqua calcis etc., and the pH value of said alkali treatment liquid can be 7～9, is good with 7.3～8; The said pretreated time can be 1～20min, is good with 8～12min.
2) pressed powder and consolidation liquid are reconciled into enamel preventing decayed tooth paint for repairing, again enamel preventing decayed tooth paint for repairing is coated on the tooth sample surfaces after, the erase residual varnish is promptly accomplished adamantine preventing decayed tooth reparation.
In step 2) in, the proportioning of said pressed powder and consolidation liquid can be 1g: (0.5～4) ml, and the proportioning of said pressed powder and consolidation liquid is preferably 1g: (1～2) ml, wherein pressed powder is calculated in mass, and the consolidation liquid by volume is calculated; The said time that enamel preventing decayed tooth paint for repairing is coated on the tooth sample surfaces can be 5～60min, is good with 10～18min.
The present invention uses acid solution that enamel surface is carried out acid etching, can remove the biomembrane that enamel surface covers, and the hydroxyapatite on the top layer of dissolving enamel, increases the roughness and the surface energy of enamel surface.With weak caustic solution enamel is carried out pretreatment subsequently, capture the hydrion of enamel surface, make the surface polarization, be more conducive to deposition with hydroxyapatite crystal.Because the hydroxyapatite in the varnish is in hypersaturated state; A large amount of hydroxyapatite is present in the varnish with the amorphous calcium phosphate form; Near between enamel crystal and the varnish at the interface because the reduction of degree of supersaturation, these calcium phosphate groups bunch are dissociated into the required ion of coated crystal growth, replenish the material that nucleation and growth consumed of coated crystal; Make the supply ion on the interface be dynamic equilibrium, coating is able to continue growth.Utilize the present invention to repair the hydroxyapatite coating layer that thickness is 10～60 μ m at enamel surface, coating combines closely with substrate, and hardness reaches more than the 170VHN.
Description of drawings
Fig. 1 is the XRD figure spectrum of resulting hydroxyapatite powder among the embodiment 1.In Fig. 1, abscissa is angle of diffraction 2Theta (degree), and vertical coordinate is diffracted intensity Intensity (a.u.).
Fig. 2 is the XRD figure spectrum of reparation preparation front and back enamel surface among the embodiment 1.In Fig. 2, abscissa is angle of diffraction 2Theta (degree), and vertical coordinate is diffracted intensity Intensity (a.u.); A is the XRD figure spectrum of preprosthetic enamel surface, and b is the XRD figure spectrum of the enamel surface after repairing.
Fig. 3 be among the embodiment 1 enamel through the Electronic Speculum picture of surface topography after the pretreatment.In Fig. 3, scale is 10 μ m.
Fig. 4 is the Electronic Speculum picture on embodiment 1 resulting reparation surface.In Fig. 4, scale is 10 μ m.
Fig. 5 is the Electronic Speculum picture of embodiment 1 resulting reparation section.In Fig. 5, scale is 50 μ m; A is an enamel, and b is a coating, and c is a resin.
The specific embodiment
Through embodiment the present invention is described further below, but these embodiment do not limit protection scope of the present invention.
Embodiment 1
With Ca (NO
3)
2H
2O (analytical pure) is dissolved in the deionized water, is made into the solution of 0.5mol/l, regulates pH value to 11 with ammonia; With (NH
4)
2HPO
4(analytical pure) is dissolved in the deionized water, is made into the solution of 0.3mol/l, regulates pH to 11 with ammonia, after stirring solution filtered.In the ratio of calcium-phosphorus ratio 1.67, calcium nitrate solution is added in the ammonium dibasic phosphate solution fast the powerful 0.5h that stirs.Mixture placed leave standstill ripening 72h under the room temperature, filter out precipitate, and wash respectively 3 times with deionized water and dehydrated alcohol.At 70 ℃ of dry 10h.With the powder porphyrize, 325 orders that sieve can obtain hydroxyapatite powder with agate mortar.Phosphoric acid with 85% mixed with 30% hydrogen peroxide in 1: 4 by volume, obtained consolidation liquid.Phosphoric acid with 37% takes out with deionized water and cleans enamel surface acid etching 30s, and the sodium hydroxide solution of reuse 0.02mol/l carries out pretreatment 10min to enamel, takes out with deionized water and cleans, dries.Take by weighing the hydroxyapatite powder of 1.5g, with the consolidation liquid uniform mixing of 2ml, process the enamel paint for repairing, rapidly this varnish is coated on enamel surface, behind the reaction 15min, the remaining varnish of flush away can obtain fine and close hydroxyapatite coating layer.
Resulting hydroxyapatite powder XRD figure is as shown in Figure 1; Can know by Fig. 1; Synthetic powder collection of illustrative plates and hydroxyapatite standard diagram (PDF#09-0432) coupling are good, and no dephasign exists, and is 31.86 °, 32.20 °, 32.90 ° 3 diffraction maximums that appearance is stronger at 2 θ; Corresponding with crystal face (211), (112) and (300) of 3 highest peaks of HA respectively, the composition that can know synthetic powder is a hydroxyapatite.
Resulting coating XRD figure spectrum is as shown in Figure 2, and the standard card (PDF#09-0432) of contrast hydroxyapatite can know that the enamel surface coating composition is a hydroxyapatite.(002) peak that coating forms the back enamel surface significantly strengthens, and explains that hydroxyapatite coating layer grows in the enamel surface preferred orientation.
Fig. 3 is pretreated enamel surface, can be known by Fig. 3, and the enamel surface pattern after surface conditioning agent is handled is lepidiod bulge-structure, and boundary is clear between enamel fiber and the enamel rod sheath.Fig. 4 is the pattern of enamel surface after repairing, and is visible by Fig. 4, the coated fully covering of enamel surface, and compact structure is smooth, no obvious defects.Fig. 5 be reparation with the section pattern behind the resin embedding, can know by Fig. 5, coating and enamel substrate seamless combination, thickness is about 25 μ m.
Embodiment 2
With Ca (NO
3)
2H
2O (analytical pure) is dissolved in the deionized water, is made into the solution of 0.5mol/l, regulates pH value to 11 with ammonia; With (NH
4)
2HPO
4(analytical pure) is dissolved in the deionized water, is made into the solution of 0.3mol/l, regulates pH to 11 with ammonia.In the ratio of calcium-phosphorus ratio 1.67, calcium nitrate solution is added in the ammonium dibasic phosphate solution fast the powerful 0.5h that stirs.Mixture placed leave standstill ripening 120h under the room temperature, filter out precipitate, and wash respectively 3 times with deionized water and dehydrated alcohol.At 70 ℃ of dry 10h.With the powder porphyrize, 325 orders that sieve can obtain hydroxyapatite powder with agate mortar.Phosphoric acid with 85% mixed with 30% hydrogen peroxide in 1: 5 by volume, obtained consolidation liquid.Phosphoric acid with 37% takes out with deionized water and cleans enamel surface acid etching 30s, and the sodium hydroxide solution of reuse 0.02mol/l carries out pretreatment 10min to enamel, takes out and cleans, dries up with deionized water.Take by weighing the hydroxyapatite of 1g, with the consolidation liquid uniform mixing of 2ml, process the enamel paint for repairing, rapidly this varnish is coated on enamel surface, behind the reaction 15min, the remaining varnish of flush away can obtain hydroxyapatite coating layer.
Embodiment 3
Phosphoric acid with 85% mixed with 30% hydrogen peroxide in 1: 4 by volume, obtained consolidation liquid., take out with deionized water and clean enamel surface acid etching 50s with saturated citric acid, the sodium hydroxide solution of reuse 0.02mol/l carries out pretreatment 10min to enamel, takes out and cleans, dries up with deionized water.Take by weighing the hydroxyapatite of 1.5g, with the consolidation liquid uniform mixing of 2ml, process the enamel paint for repairing, rapidly this varnish is coated on enamel surface, behind the reaction 15min, the remaining varnish of flush away can obtain hydroxyapatite coating layer.
Embodiment 4
Phosphoric acid with 85% mixed with 30% hydrogen peroxide in 1: 4 by volume, obtained consolidation liquid., take out with deionized water and clean enamel surface acid etching 50s with saturated citric acid, the aqua calcis of reuse 0.01mol/l carries out pretreatment 20min to enamel, takes out and cleans, dries up with deionized water.Take by weighing the hydroxyapatite of 1.5g, with the consolidation liquid uniform mixing of 2ml, process the enamel paint for repairing, rapidly this varnish is coated on enamel surface, behind the reaction 15min, the remaining varnish of flush away can obtain hydroxyapatite coating layer.
Claims (3)
1. an enamel preventing decayed tooth paint for repairing is characterized in that comprising pressed powder and consolidation liquid, and said pressed powder is a hydroxyapatite powder, and said consolidation liquid is at least a in phosphoric acid, the hydrogen peroxide;
The calcium-phosphorus ratio of said hydroxyapatite powder is 1.67;
The particle diameter of said hydroxyapatite powder is 5～40 μ m;
Said consolidation liquid is the mixed solution of phosphoric acid and hydrogen peroxide, and in the mixed solution of phosphoric acid and hydrogen peroxide, the volume ratio of phosphoric acid and hydrogen peroxide is (0.1～0.5): 1.
2. a kind of enamel preventing decayed tooth paint for repairing as claimed in claim 1, the particle diameter that it is characterized in that said hydroxyapatite powder is 5～20 μ m.
3. a kind of enamel preventing decayed tooth paint for repairing as claimed in claim 1, the mass percent concentration that it is characterized in that said phosphoric acid is 85%, the mass percent concentration of said hydrogen peroxide is 30%.
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| CN2011102035177A CN102274127B (en) | 2011-07-20 | 2011-07-20 | Tooth enamel caries prevention repair coating agent and use method thereof |
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| CN2011102035177A CN102274127B (en) | 2011-07-20 | 2011-07-20 | Tooth enamel caries prevention repair coating agent and use method thereof |
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| CN102274127B true CN102274127B (en) | 2012-11-14 |
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| CN106806152A (en) * | 2017-01-22 | 2017-06-09 | 桂林碳谷科技有限公司 | A kind of biological preventing decayed tooth teeth repairing material and preparation method thereof |
| CN115006263B (en) * | 2022-06-24 | 2024-03-26 | 深圳市恒通栢能实业有限公司 | Enamel restoration material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103053A (en) * | 1993-08-19 | 1995-05-31 | 皇星技术(英国)有限公司 | Hydroxyapatite as bone or tooth replacement |
| CN1965780A (en) * | 2006-10-30 | 2007-05-23 | 厦门大学 | Paint for repairing early-stage caries on enamel surface |
| CN101810540A (en) * | 2010-04-06 | 2010-08-25 | 厦门大学 | Composition for tooth-surface anticaries repair and preparation method thereof |
-
2011
- 2011-07-20 CN CN2011102035177A patent/CN102274127B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103053A (en) * | 1993-08-19 | 1995-05-31 | 皇星技术(英国)有限公司 | Hydroxyapatite as bone or tooth replacement |
| CN1965780A (en) * | 2006-10-30 | 2007-05-23 | 厦门大学 | Paint for repairing early-stage caries on enamel surface |
| CN101810540A (en) * | 2010-04-06 | 2010-08-25 | 厦门大学 | Composition for tooth-surface anticaries repair and preparation method thereof |
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