CN106821768A - A kind of photocuring biology preventing decayed tooth teeth repairing material and preparation method thereof - Google Patents

A kind of photocuring biology preventing decayed tooth teeth repairing material and preparation method thereof Download PDF

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Publication number
CN106821768A
CN106821768A CN201710047695.2A CN201710047695A CN106821768A CN 106821768 A CN106821768 A CN 106821768A CN 201710047695 A CN201710047695 A CN 201710047695A CN 106821768 A CN106821768 A CN 106821768A
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China
Prior art keywords
solution
photocuring
repairing material
preparation
decayed tooth
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CN201710047695.2A
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CN106821768B (en
Inventor
王宏
潘自立
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GUANGXI NAWEI ANGEL MEDICAL EQUIPMENT Co.,Ltd.
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Guilin Carbon Valley Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/831Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
    • A61K6/838Phosphorus compounds, e.g. apatite
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/884Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
    • A61K6/887Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds

Abstract

The present invention discloses a kind of photocuring biology preventing decayed tooth teeth repairing material and preparation method thereof, comprises the following steps:1, it is 10 30% ethanol solution using acetic acid volume fraction, and pH value of solution to 35 is adjusted, obtain solution A;2, the surface modifier KH 570 of gross mass 1 2.5%, i.e. γ methacryloxypropyl trimethoxy silanes are added in the solution A, obtain solution B;3, in solution B add fluorine hydroxyapatite, ultrasonic reaction 14 hours, after 0.5 2h is reacted at 50 80 DEG C, while stirring, by sediment washing, dry after grind, obtain solid phase C;4, the Bis GMA of different proportion, i.e. resin bisphenol-A GMA and TEGDMA, i.e. TEGDMA organic matter monomer are configured, acetone soln is dissolved in, obtain solution D;5, camphorate quinone and DMAEMA in the solution D, obtains solution E;6, the solid phase C is added in the solution E, stir, ultraviolet light polymerization obtains target product.

Description

A kind of photocuring biology preventing decayed tooth teeth repairing material and preparation method thereof
Technical field
The present invention relates to teeth repairing material field, and in particular to a kind of photocuring biology preventing decayed tooth teeth repairing material and its Preparation method.
Background technology
Teeth repairing material plays vital effect in the reparation of tooth.Metal and non-is broadly divided into by its attribute The class of metal two;Metal class is main based on silver amalgam and titanium alloy, and non-metal kind is mainly with hydroxyapatite and compound tree Fat is representative.Human body fluid Long Term Contact metal class teeth repairing material can produce corrosion to it, cause metal ion and its spread out Biology is separated out, and this can produce certain injury to organism tissue, such as locally or systemically poisoning, allergic reaction.Hydroxy-apatite Stone is a kind of calcium salt of the alkalescent phosphoric acid for being slightly soluble in water, is also the main inorganic composition of human body hard tissue, is presently believed to be A kind of best bio-medical material for substituting human body hard tissue.But itself also has certain defect, such as solubility High, fragility than larger, biomechanical strength and the more low problems of antifatigue breakdown strength.Light-cured resin is wide now The general material for being applied to Dental Erosion, its random defect that can quickly repair dental tissue, but anti-wear performance is poor, should not hold By larger masticatory force, this severely limits its teeth repairing material field application.Find preferable teeth repairing material one It is directly the focus of oral cavity biomedical materials field research.
Fluorine ion is widely used in biological dopant material due to its unique physical and chemical performance and biological agent. Fluorine ion can improve the physicochemical properties of material, such as dissolubility, structure, mechanical characteristic.Additionally, the release of fluorine ion can also The preventing decayed tooth performance of enhancing dentine and enamel.Numerous studies show that Fluorin doped is carried out to hydroxyapatite can obtain more excellent Biomechanical strength.
In view of drawbacks described above, creator of the present invention passes through prolonged research and practice obtains the present invention finally.
The content of the invention
To solve above-mentioned technological deficiency, the technical solution adopted by the present invention is, there is provided a kind of photocuring biology preventing decayed tooth tooth The preparation method of tooth repair materials, comprises the following steps:
The first step, is the ethanol solution of 10-30% using acetic acid volume fraction, and adjusts pH value of solution to 3-5, is obtained Solution A;
Second step, adds the surface modifier KH-570 of gross mass 1-2.5%, i.e. γ-metering system in the solution A Acryloxypropylethoxysilane trimethoxy silane, obtains solution B;
3rd step, in solution B add fluorine hydroxyapatite, ultrasonic reaction 1-4 hour, after at 50-80 DEG C reaction 0.5-2h, while stirring, will grind after sediment washing, drying, obtains solid phase C;
4th step, configure different proportion Bis-GMA, i.e., resin bisphenol-A-GMA with TEGDMA, i.e. TEGDMA organic matter monomer, are dissolved in acetone soln, obtain solution D;
5th step, camphorate quinone and DMAEMA in the solution D, obtains solution E;
6th step, adds the solid phase C in the solution E, stirs, and ultraviolet light polymerization obtains target product.
Preferably, the mass ratio of the Bis-GMA and TEGDMA is 4:1~1:1.
Preferably, the addition of the fluorine hydroxyapatite is 5-10%.
Preferably, a length of 200~400nm of ultraviolet light wave, irradiation time is 1~3min, and luminous intensity is 50~300mW/ cm2。
Preferably, providing photocuring biology preventing decayed tooth teeth repairing material prepared by the method described in any of the above.
Compared with the prior art the beneficial effects of the present invention are:1) photocuring biology preventing decayed tooth teeth repairing material is prepared Raw material is easy to get;2) preparation process is simple;3) physical and mechanical properties of the biological preventing decayed tooth teeth repairing material for preparing is excellent and has Certain preventing decayed tooth function;4) random defect of dental tissue can quickly be repaired.
Specific embodiment
The technical characteristic above-mentioned and other to the present invention and advantage are described in more detail.
Embodiment 1
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 25% is to pH to 4 or so;
2. the KH-570 of 2mg is added;
3. the fluorine hydroxyapatite of 10mg, ultrasonic 1h are added;
4. continue under the conditions of 50 DEG C to stir 2h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 6g Bis-GMA and 4g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 10g modified stirs;
9. luminous intensity is the 365nm ultra violet lamps 1min solidifications of 200mW/cm2.
Embodiment 2
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 10% is to pH to 3 or so;
2. the KH-570 of 2.5mg is added;
3. the fluorine hydroxyapatite of 10mg, ultrasonic 2h are added;
4. continue under the conditions of 60 DEG C to stir 1h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 4g Bis-GMA and 2g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 5g modified stirs;
9. luminous intensity is the 400nm ultra violet lamps 2min solidifications of 200mW/cm2.
Embodiment 3
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 30% is to pH to 5 or so;
2. the KH-570 of 1mg is added;
3. the fluorine hydroxyapatite of 10mg, ultrasonic 4h are added;
4. continue under the conditions of 80 DEG C to stir 4h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 1g Bis-GMA and 1g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 10g modified stirs;
9. luminous intensity is the 265nm ultra violet lamps 3min solidifications of 200mW/cm2.
Embodiment 4
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 15% is to pH to 4 or so;
2. the KH-570 of 1.5mg is added;
3. the fluorine hydroxyapatite of 5mg, ultrasonic 2h are added;
4. continue under the conditions of 70 DEG C to stir 1h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 4g Bis-GMA and 1g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 7g modified stirs;
9. luminous intensity is the 2005nm ultra violet lamps 3min solidifications of 200mW/cm2.
Embodiment 5
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 15% is to pH to 4 or so;
2. the KH-570 of 2mg is added;
3. the fluorine hydroxyapatite of 10mg, ultrasonic 1h are added;
4. continue under the conditions of 50 DEG C to stir 2h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 6g Bis-GMA and 4g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 10g modified stirs;
9. luminous intensity is the 365nm ultra violet lamps 1min solidifications of 300mW/cm2.
Embodiment 6
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 10% is to pH to 2 or so;
2. the KH-570 of 1mg is added;
3. the fluorine hydroxyapatite of 8mg, ultrasonic 1h are added;
4. continue under the conditions of 50 DEG C to stir 4h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 4g Bis-GMA and 4g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 10g modified stirs;
9. luminous intensity is the 365nm ultra violet lamps 1min solidifications of 50mW/cm2.
Embodiment 7
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 17% is to pH to 4 or so;
2. the KH-570 of 2.5mg is added;
3. the fluorine hydroxyapatite of 10mg, ultrasonic 4h are added;
4. continue under the conditions of 80 DEG C to stir 2h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 3g Bis-GMA and 1g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 10g modified stirs;
9. luminous intensity is the 365nm ultra violet lamps 1min solidifications of 350mW/cm2.
Embodiment 8
The preparation method of photocuring biology preventing decayed tooth teeth repairing material includes following steps:
1. the ethanol water of acetic acid 100ml 10% is to pH to 4 or so;
2. the KH-570 of 1mg is added;
3. the fluorine hydroxyapatite of 20mg, ultrasonic 1h are added;
4. continue under the conditions of 80 DEG C to stir 2h;
5. deionized water is fully washed, and room temperature in vacuo dries , Yan Portland grindings;
6. 2g Bis-GMA and 1g TEGDMA are dissolved in 50ml acetone solns;
7. 800mg camphorquinones and 800mg DMAEMA are added;
8. the fluorine hydroxyapatite for adding 10g modified stirs;
9. luminous intensity is the 365nm ultra violet lamps 1min solidifications of 2800mW/cm2.
Embodiment 11
The fluorine-ion-doped mass fraction is repaired the follow-up dental caries of tooth after tooth wedge lacks and is damaged with fluorine hydroxyapatite material There is following relation in degree:
Y=3.03x2-0.983x+0.167(0≥X≥0.08)
Wherein, the follow-up dental caries of tooth damage degree after y lacks for fluorine hydroxyapatite material reparation tooth wedge, and unit is mm, and x is to add Enter the fluorine ion percentage.In general, various equivalent modifications are in order to determine hydroxyl of the tooth to different Oil repellents Preventing decayed tooth situation under base Apatite materials is sampled contrast, is then tested by complicated instrument again, and test process is multiple It is miscellaneous and expensive, it is necessary to repeated multiple times experiment determines, waste human and material resources, time and resource.But it is public more than Formula, in the case where experiment condition is certain, it is only necessary to determine Oil repellent, it is possible to obtain the journey that follow-up tooth further corrodes Degree, according to the different situations of personal tooth quality, is calculated by simple formula, the doping of fluorine in adjustment hydroxyapatite, It is time saving and energy saving.
Presently preferred embodiments of the present invention is the foregoing is only, is merely illustrative for the purpose of the present invention, and it is non-limiting 's.Those skilled in the art understanding, many changes can be carried out in the spirit and scope that the claims in the present invention are limited to it, Modification, in addition it is equivalent, but fall within protection scope of the present invention.

Claims (5)

1. the preparation method of a kind of photocuring biology preventing decayed tooth teeth repairing material, it is characterised in that comprise the following steps:
The first step, is the ethanol solution of 10-30% using acetic acid volume fraction, and adjusts pH value of solution to 3-5, obtains solution A;
Second step, adds the surface modifier KH-570 of gross mass 1-2.5%, i.e. γ-methacryloxypropyl in the solution A Base propyl trimethoxy silicane, obtains solution B;
3rd step, in solution B add fluorine hydroxyapatite, ultrasonic reaction 1-4 hours, after react 0.5-2h at 50-80 DEG C, Simultaneously stir, by sediment washing, dry after grind, obtain solid phase C;
4th step, configures the Bis-GMA of different proportion, i.e. resin bisphenol-A-GMA and TEGDMA, i.e., TEGDMA organic matter monomer, is dissolved in acetone soln, obtains solution D;
5th step, camphorate quinone and DMAEMA in the solution D, obtains solution E;
6th step, adds the solid phase C in the solution E, stirs, and ultraviolet light polymerization obtains target product.
2. a kind of preparation method of photocuring biology preventing decayed tooth teeth repairing material as claimed in claim 1, it is characterised in that institute The mass ratio for stating Bis-GMA and TEGDMA is 4:1~1:1.
3. a kind of preparation method of photocuring biology preventing decayed tooth teeth repairing material as claimed in claim 2, it is characterised in that institute The addition for stating fluorine hydroxyapatite is 5-10%.
4. the preparation method of a kind of photocuring biology preventing decayed tooth teeth repairing material as claimed in claim 3, it is characterised in that purple The outer a length of 200~400nm of light wave, irradiation time is 1~3min, and luminous intensity is 50~300mW/cm2.
5. any described method of Claims 1 to 4 prepares photocuring biology preventing decayed tooth teeth repairing material.
CN201710047695.2A 2017-01-22 2017-01-22 Photo-curing biological anti-caries tooth repair material and preparation method thereof Active CN106821768B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110606913A (en) * 2019-09-11 2019-12-24 国网吉林省电力有限公司电力科学研究院 Acrylate material capable of being rapidly cured by visible light and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070155853A1 (en) * 2005-12-29 2007-07-05 Xiangxu Chen One-component dental adhesive compositions and method of use
CN101564357A (en) * 2009-06-02 2009-10-28 李榕卿 Photo-curing composition for tooth
CN101669885A (en) * 2009-08-17 2010-03-17 李榕卿 Dental material reinforced by rigid inorganic nano-filler
CN103637919A (en) * 2013-12-04 2014-03-19 东华大学 Preparation method of sea urchin type hydroxyapatite-reinforced dental repair resin
CN103919686A (en) * 2013-01-11 2014-07-16 王青山 Tooth repair nanometer hydroxyapatite composite material and preparation method thereof
CN105496797A (en) * 2015-12-14 2016-04-20 天津君润新材料科技有限公司 Photo-curable anti-caries fluoride coating film

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070155853A1 (en) * 2005-12-29 2007-07-05 Xiangxu Chen One-component dental adhesive compositions and method of use
CN101564357A (en) * 2009-06-02 2009-10-28 李榕卿 Photo-curing composition for tooth
CN101669885A (en) * 2009-08-17 2010-03-17 李榕卿 Dental material reinforced by rigid inorganic nano-filler
CN103919686A (en) * 2013-01-11 2014-07-16 王青山 Tooth repair nanometer hydroxyapatite composite material and preparation method thereof
CN103637919A (en) * 2013-12-04 2014-03-19 东华大学 Preparation method of sea urchin type hydroxyapatite-reinforced dental repair resin
CN105496797A (en) * 2015-12-14 2016-04-20 天津君润新材料科技有限公司 Photo-curable anti-caries fluoride coating film

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110606913A (en) * 2019-09-11 2019-12-24 国网吉林省电力有限公司电力科学研究院 Acrylate material capable of being rapidly cured by visible light and preparation method thereof
CN110606913B (en) * 2019-09-11 2021-06-04 国网吉林省电力有限公司电力科学研究院 Acrylate material capable of being rapidly cured by visible light and preparation method thereof

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