CN102961259A - Hard coating material used for dental restoration and preparation method thereof - Google Patents
Hard coating material used for dental restoration and preparation method thereof Download PDFInfo
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- CN102961259A CN102961259A CN2012105346897A CN201210534689A CN102961259A CN 102961259 A CN102961259 A CN 102961259A CN 2012105346897 A CN2012105346897 A CN 2012105346897A CN 201210534689 A CN201210534689 A CN 201210534689A CN 102961259 A CN102961259 A CN 102961259A
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- repair liquid
- fluoride
- ethylenediaminetetraacetic acid
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Abstract
The invention relates to a fluoro-apatite hard coating material used for dental restoration and a preparation technology thereof. Raw materials comprise a water soluble ethylene diamine tetraacetic acid metal salt, monocalcium phosphate, a water soluble fluoride and an alkaline compound. The preparation technology comprises the following steps of: 1) preparing restoration solution, comprising the steps of adding certain amount of water soluble ethylene diamine tetraacetic acid metal salt and monocalcium phosphate into aqueous solution at the same time, then adding the alkaline compound in certain proportion to regulate pH value of a system to be an expected value, fully dissolving to obtain a saturated suspension, then filtering, reserving transparent filtrate and adding the water soluble fluoride in certain proportion into the filtrate; and 2) applying the restoration solution to a dental enamel base or a prophase carious dental enamel part, and thus obtaining the fluoro-apatite hard coating material on the surface of the dental enamel base or the prophase carious dental enamel part after a period of time. The coating material is tightly connected with the dental enamel base, hardness of the coating material is better than that of a natural tooth, the coating material can realize the effects of solidifying dental enamel and protecting teeth, a synthetic process of the coating material is simple, reaction conditions are mild, and the coating material is hopeful to be applied to the fields of toothpaste, mouthwash and dentistry clinical restoration, especially prevention and treatment of prophase caries and pit and fissure sealing.
Description
Technical field
The present invention relates to a kind of dental prosthetic material, especially relate to a kind of fluorine-based apatite hard coating material and technology of preparing thereof for the enamel reparation.
Background technology
Enamel has unique multilevel hierarchy as height mineralized tissue the hardest in the vertebrates body, makes it have excellent mechanics and biomedical protective value.The present balance that in adamantine surperficial oral environment, exists demineralization and remineralization that studies show that, think dental caries be since cariogenic bacteria, tooth host, fermentable carbohydrate and time factor combined effect so that the mineral demineralization in the enamel is decomposed causes.
The main method of the at present clinical treatment early stage caries of generally using is pit and fissure sealant preventing decayed tooth and filling treatment.The composition of pit and fissure sealant is coated it on the nest ditch of crossing through acid etching take composite resin material as main, thus the generation of caries prevention.But there is following shortcoming in composite resin: (a) wearability is relatively poor; (b) polymerization shrinkage is larger, has increased the probability of recurrent caries; (c) linear expansion coefficient is greater than natural teeth; (d) polymerization is incomplete, has residual monomer, and residual monomer affects mechanical performance and biology performance; Fatigue phenomenon appears in (e) composite resin easily degraded in oral environment.Behind the nest ditch closed treating, the check of must making regular check on or send for a doctor, sealer is if any coming off, the closed treating of should sending for a doctor to re-start.
The basic process of filling technique can be divided into for two steps: machinery is removed bad position of dental caries first, makes reasonable nest hole form; Fill with filler, and recover the profile of tooth defect.During the bad treatment of dental caries, depending on the circumstances or the needs of the situation at the bottom of the hole, add one deck and protect that the marrow agent recharges or first to endodontic treatment, then could fill.Filler mainly contains silver amalgam, glass, composite resin, zinc oxide clove oil cement flour, calcium phosphate bone cement powder, portland cement powder etc.The shortcoming of this method is: (a) physicochemical property of filler is different from enamel itself, and the two adhesion is not good, and biocompatibility is bad, the material coefficient of expansion difference generation recurrent caries that comes off easily; (b) need to remove unnecessary healthy tooth part, so that cavity further enlarges.Therefore find a kind of safely and effectively dental caries repair materials, have great clinical value.
Crystal structure and the hydroxyapatite of fluorine-based apatite are similar, all belong to hexagonal crystal system, and just the position of hydroxyapatite hydroxyl is partly or entirely replaced by fluorine.We know 96%～97% of tooth gross mass, and inorganic material mainly is hydroxyapatite, and major part exists with crystalline state.A large amount of studies show that the crystal structure of fluorine-based apatite is more stable than hydroxyapatite, so its hardness also is higher than hydroxyapatite.
Summary of the invention
The present invention seeks to prepare a kind of fluorine-based apatite hard coating material, be used for the front dental caries reparation control of dentistry, and improve tooth hardness, play the effect that firm enamel takes care of one's teeth.The technology of preparing of fluorine-based apatite hard coating material of the present invention, concrete steps are as follows:
1) repair liquid preparation: in aqueous solution, add a certain amount of water solublity ethylenediaminetetraacetic acid slaine and dalcium biphosphate, and add alkali compounds regulation system pH to expected value, fully dissolving makes saturated suspension, then filter the transparent filtrate of reservation, in filtrate, add a certain proportion of fluoride;
2) above-mentioned saturated repair liquid is acted on the enamel position of enamel substrate or front dental caries, obtain fluorine-based apatite hard coating material at enamel surface in the certain environment temperature after insulation a period of time.
Described water solublity ethylenediaminetetraacetic acid slaine can be a kind of in disodium EDTA, sodium versenate salt, tetrasodium salt of EDTA, EDTA Dipotassium salt, calcium disodium chelate salt, the ethylenediamine tetraacetic acid disodium magnesium salt salt.
Described dalcium biphosphate can be a kind of in a hypophosphite monohydrate calcium dihydrogen, the anhydrous dihydro calcium phosphate.
The addition ratio of described ethylenediaminetetraacetic acid slaine, 0.01mol～0.5mol(ethylenediaminetetraacetic acid slaine): the total solution of 1L(), wherein take 0.1mol～0.2mol(ethylenediaminetetraacetic acid slaine): the total solution of 1L() as good.
The addition ratio of described dalcium biphosphate, 0.01mol～0.5mol(dalcium biphosphate): the total solution of 1L(), wherein take 0.08mol～0.2mol(dalcium biphosphate): the total solution of 1L() as good.
The alkali compounds that described adjustment system pH is used can be NaOH, KOH, NH
4A kind of among the OH, the desired pH scope of repair liquid is 4.0～9.0, wherein take 5.0～7.0 as good.
Described fluoride can be a kind of in sodium fluoride, potassium fluoride, the ammonium fluoride, and its addition ratio is 0.01mol～0.05mol(sodium fluoride): the total solution of 1L().
Described when repair liquid is acted on the enamel position of enamel substrate or front dental caries, its ambient temperature is 10 ℃～60 ℃, wherein take 30 ℃～40 ℃ as good.
Described when repair liquid is acted on the enamel position of enamel substrate or front dental caries, be 2 hours～10 days its action time, wherein take 1 day～5 days as good.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) picture of experiment labial teeth MICROSCOPY SURFACE TOPOGRAPHY OF HUMAN ENAMEL.
Fig. 2 is the SEM picture of the rear enamel surface coating material of experiment.
Fig. 3 is the component analysis X ray energy dispersion spectrum (EDS) of coating material.
Fig. 4 is that the X ray diffracting spectrum (XRD) of enamel surface compares before and after the coating material growth, and abscissa is the angle of diffraction 2 Theta in the drawings, and vertical coordinate is relative diffracted intensity Intensity(a.u.).
The specific embodiment
Embodiment 1
Prepare the tooth sample, provide and allow through patient by hospital, at first enamel is carried out dental caries simulation in early stage, be that 37% phosphoric acid etching agent carried out pretreatment 30 seconds to enamel surface with solubility, then wash with water clean, pattern as shown in Figure 1, rough surface presents the dentium nitor post that diameter is about 5 μ m.
Measure the 100mL deionized water, add the disodiumedetate of 0.01mol and the anhydrous dihydro calcium phosphate of 0.01mol, the potassium hydroxide solution regulation system pH value that drips 5mol/L is stabilized in 6.0, fully stirring and dissolving makes saturated suspension in 80 ℃ of environment, then filters to keep transparent filtrate.Measure the above-mentioned transparent filtrate of 50mL, add the sodium fluoride of 0.001mol, namely get repair liquid.
Above-mentioned tooth sample is placed above-mentioned repair liquid, and in 37 ℃ of temperature normal pressure heat-insulatings 5 days, take out water and rinse well, characterize by experiment and confirm to obtain fluorine-based apatite coating at enamel surface.
This coating pattern as shown in Figure 2, the hexagonal of closely arranging, its single crystal width is about 300nm.Fig. 3 is that X ray energy dispersion spectrum (EDS) is carried out the coating composition analysis, finds to have significant fluorine element to exist, and characterizes in conjunction with the XRD phase, judges that the coating phase is fluorine-based apatite phase.Before and after the experiment of Fig. 4 XRD contrast collection of illustrative plates as can be known, at first crystal phase and the enamel of reparation are similar, similar so coating and substrate have good adhesion owing to the structure of matter; Secondly the degree of crystallinity of coating will be higher than the enamel substrate; Coated crystal is that what finally present is (001) hexagonal crystal face along the growth of c-axis direction preferred orientation again.
The coating microhardness test result is as follows, and hardness reaches 338.7HV, has improved 57.9% before repairing.
| Sample | 1st/HV | 2nd/HV | 3rd/HV | Average/HV | Standard Deviation/HV |
| Before the reparative experiment | 219.6 | 213.3 | 210.4 | 214.4 | 4.7 |
| Behind the reparative experiment | 344.3 | 339.2 | 332.7 | 338.7 | 5.8 |
Embodiment 2
Measure the 100mL deionized water, add the ethylenediamine tetraacetic acid,dipotassium salt of 0.01mol and the anhydrous dihydro calcium phosphate of 0.01mol, the potassium hydroxide solution regulation system pH value that drips 5mol/L is stabilized in 7.0, fully stirring and dissolving makes saturated suspension in 80 ℃ of environment, then filters to keep transparent filtrate.Measure the above-mentioned transparent filtrate of 50mL, add the sodium fluoride of 0.001mol, namely get repair liquid.
Above-mentioned tooth sample is placed above-mentioned repair liquid, and in 30 ℃ of temperature normal pressure heat-insulatings 10 days, take out water and rinse well, obtain fluorine-based apatite coating at enamel surface.
Embodiment 3
Measure the 100mL deionized water, add the sodium versenate of 0.5mol and the hypophosphite monohydrate calcium dihydrogen of 0.1mol, the potassium hydroxide solution regulation system pH value that drips 5mol/L is stabilized in 6.0, fully stirring and dissolving makes saturated suspension in 50 ℃ of environment, then filters to keep transparent filtrate.Measure the above-mentioned transparent filtrate of 50mL, add the sodium fluoride of 0.003mol, namely get repair liquid.
Above-mentioned tooth sample is placed above-mentioned repair liquid, and in 37 ℃ of temperature normal pressure heat-insulatings 1 day, take out water and rinse well, obtain fluorine-based apatite coating at enamel surface.
Embodiment 4
Measure the 100mL deionized water, add the tetrasodium ethylenediamine tetraacetate of 0.005mol and 0.01mol without the hydration dalcium biphosphate, the potassium hydroxide solution regulation system pH value that drips 5mol/L is stabilized in 5.0, fully stirring and dissolving makes saturated suspension in 80 ℃ of environment, then filters to keep transparent filtrate.Measure the above-mentioned transparent filtrate of 50mL, add the sodium fluoride of 0.001mol, namely get repair liquid.
Above-mentioned tooth sample is placed above-mentioned repair liquid, and in 40 ℃ of temperature normal pressure heat-insulatings 6 hours, take out water and rinse well, obtain fluorine-based apatite coating at enamel surface.
Embodiment 5
Measure the 100mL deionized water, add the ethylenediamine tetraacetic acid,dipotassium salt of 0.01mol and the hypophosphite monohydrate calcium dihydrogen of 0.01mol, the potassium hydroxide solution regulation system pH value that drips 5mol/L is stabilized in 6.0, fully stirring and dissolving makes saturated suspension in 60 ℃ of environment, then filters to keep transparent filtrate.Measure the above-mentioned transparent filtrate of 50mL, add the sodium fluoride of 0.002mol, namely get repair liquid.
Above-mentioned tooth sample is placed above-mentioned repair liquid, and in 40 ℃ of temperature normal pressure heat-insulatings 2 hours, take out water and rinse well, obtain fluorine-based apatite coating at enamel surface.
Claims (9)
1. hard coating material that is used for dental prosthetic and preparation method thereof may further comprise the steps:
1) repair liquid preparation: in aqueous solution, add a certain amount of water solublity ethylenediaminetetraacetic acid slaine and dalcium biphosphate, and add alkali compounds regulation system pH to expected value, fully dissolving makes saturated suspension, then filter the transparent filtrate of reservation, in filtrate, add a certain proportion of fluoride;
2) above-mentioned saturated repair liquid is acted on the enamel position of enamel substrate or front dental caries, obtain fluorine-based apatite hard coating material at enamel surface in the certain environment temperature after insulation a period of time.
2. method according to claim 1, it is characterized in that described water solublity ethylenediaminetetraacetic acid slaine, can be a kind of in disodium EDTA, sodium versenate salt, tetrasodium salt of EDTA, EDTA Dipotassium salt, calcium disodium chelate salt, the ethylenediamine tetraacetic acid disodium magnesium salt salt.
3. method according to claim 1 is characterized in that described dalcium biphosphate, can be a kind of in a hypophosphite monohydrate calcium dihydrogen, the anhydrous dihydro calcium phosphate.
4. method according to claim 1, the addition ratio that it is characterized in that described ethylenediaminetetraacetic acid slaine, 0.01mol～0.5mol(ethylenediaminetetraacetic acid slaine): the total solution of 1L(), wherein take 0.1mol～0.2mol(ethylenediaminetetraacetic acid slaine): the total solution of 1L() as good.
5. method according to claim 1, the addition ratio that it is characterized in that described dalcium biphosphate, 0.01mol～0.5mol(dalcium biphosphate): the total solution of 1L(), wherein take 0.08mol～0.1mol(ethylenediaminetetraacetic acid slaine): the total solution of 1L() as good.
6. method according to claim 1, it is characterized in that described is alkali compounds for what regulate the repair liquid system pH, can be NaOH, KOH, NH
4A kind of among the OH, the desired pH scope of repair liquid is 4.0～9.0, wherein take 5.0～7.0 as good.
7. method according to claim 1 is characterized in that described fluoride, can be a kind of in sodium fluoride, potassium fluoride, the ammonium fluoride, and its addition ratio is 0.01mol～0.05mol(sodium fluoride): the total solution of 1L().
8. method according to claim 1 is characterized in that describedly when repair liquid is acted on the enamel position of enamel substrate or front dental caries, and its ambient temperature is 10 ℃～60 ℃, wherein take 30 ℃～40 ℃ as good.
9. method according to claim 1 is characterized in that describedly when repair liquid is acted on the enamel position of enamel substrate or front dental caries, and be 2 hours～10 days its action time, wherein take 1 day～5 days as good.
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Application publication date: 20130313 |