CN108245433A - A kind of novel mouth section glass ionomer/fluorinated graphene composite material - Google Patents

A kind of novel mouth section glass ionomer/fluorinated graphene composite material Download PDF

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Publication number
CN108245433A
CN108245433A CN201711390207.4A CN201711390207A CN108245433A CN 108245433 A CN108245433 A CN 108245433A CN 201711390207 A CN201711390207 A CN 201711390207A CN 108245433 A CN108245433 A CN 108245433A
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CN
China
Prior art keywords
fluorinated graphene
glass ionomer
ethyl alcohol
glass
composite material
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Pending
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CN201711390207.4A
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Chinese (zh)
Inventor
张俊彦
孙莉
刘斌
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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Priority to CN201711390207.4A priority Critical patent/CN108245433A/en
Publication of CN108245433A publication Critical patent/CN108245433A/en
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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
    • A61K6/836Glass
    • 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

Abstract

The invention discloses a kind of novel mouth section glass ionomer/fluorinated graphene composite materials.The present invention is uniformly mixed the two using the method that mechanical ultrasonic is blended using conventional glass-ionomer cement pulvis common in clinical oral and fluorinated graphene as raw material.The two is dispersed in absolute ethyl alcohol by a certain percentage, ultrasound promotes its dispersion, and grinding is uniform and ethyl alcohol is made to volatilize completely, obtains novel dental material --- glass ionomer and fluorinated graphene mixing powder.Preparation method of the present invention is simple, equipment is simple, cheap, easy to promote large-scale.Novel dental material prepared by the present invention has high microhardness, high compression-strength, high-wearing feature, high anti-microbial property, with the color and luster for influencing material frequently, Fluoride release performance and dissolubility.The quality of filler can significantly be improved, expanded glass ionomer in clinical application range.

Description

A kind of novel mouth section glass ionomer/fluorinated graphene composite material
Technical field
The invention belongs to medical high polymer technical fields, are related to a kind of novel mouth section glass ionomer/fluorination stone Black alkene composite material.
Background technology
Glass ionomer is a kind of clinically used repair materials of department of stomatology.It is invented from last century the seventies After coming, because it is with long-term fluorine releasability, good caking property and biocompatibility, smaller plup stimulus, with tooth The near coefficient of thermal expansion of toe joint and translucent white colored appearance are widely used in restoration of tooth, fissure blockade, rebasing, glue All various aspects of the clinical orals such as knot.But for a long time, since the mechanical strength of glass ionomer is low, brittleness is big, wear-resisting Property is poor, the defects of to water sensitive, it is made to be difficult to bear the larger stress in backteeth area and long-term oral restoration.In Clinical practice, often Dummy is caused to come off in short term, the generation of secondary caries seriously limits the further extensive use of glass ionomer.Institute To improve its mechanical performance, it is the hot spot being modified to glass ionomer to enhance wearability and antibiotic property.Previous research is led to It crosses and is changed to glass ionomer pulvis addition metal, hydroxyapatite, resin, glass fibre, inorganic nano-particle etc. Property.However, the addition of metal can influence the color and luster of artificial tooth, the practicality is reduced;Resin compounded glass ionomer possess compared with Good mechanical performance and antilysis, but the addition of resin can influence its Fluoride release, and polymerize caused by resin polymerization The bonding of tissue can be influenced by shrinking;Its mechanical performance can be enhanced, but manufacture craft is more demanding by adding in glass fibre, be industrialized Production is difficult;The addition of hydroxyapatite can effectively improve its biological property, but mechanical performance is not improved;Nano-particle Filler mainly has nano-titanium dioxide, nano zirconium dioxide, nanometer fluor-apatite etc., these particles easily occur to reunite so as to make The advantages of nano material, cannot show well.
Graphene has excellent heat conduction, conductive and mechanical properties, while has good biocompatibility, thermal stability And chemical stability, in recent years by the concern of material circle.Fluorinated graphene not only retains as a kind of derivative of graphene The good characteristic of graphene, such as mechanical performance, antibiotic property etc., and with its peculiar property.It is low with polarity, hydrophobic to dredge The characteristics of oily, while fluorinated graphene is white, dispersion liquid is transparent, and does not influence the color and luster of material.
Invention content
The object of the present invention is to provide a kind of novel mouth section glass ionomer/fluorinated graphene composite materials.
A kind of novel mouth section glass ionomer/fluorinated graphene composite material, it is characterised in that the composite material It is prepared by the following method to obtain:
1)Fluorinated graphene powder is added in the dispersion solution of the ultrasonic absolute ethyl alcohol for obtaining fluorinated graphene in absolute ethyl alcohol;
2)By glass ionomer pulvis add in fluorinated graphene absolute ethyl alcohol dispersion solution in, ultrasound obtain glass from Sub- cement and fluorinated graphene dispersion solution, it grinds in mortar uniformly, after making ethyl alcohol volatilization complete, obtain glass from Sub- cement and fluorinated graphene mixing powder;
3)Mixing powder and glass ionomer liquor tune are mixed, novel artificial tooth packing material is obtained after its curing.
The mass ratio of the mixing powder and glass ionomer liquor is 2:1.
Fluorinated graphene is added in conventional glass-ionomer cement pulvis by the present invention, has prepared novel dentistry Filler makes its conventional glass-ionomer cement than current Clinical practice have more excellent mechanical strength, wear-resisting Property, stronger antibiotic property, the Fluoride release ability of longer time, so as to delay the formation of secondary caries, and it is in beautiful color, face Bed is highly practical.
Description of the drawings
Fig. 1 is the microhardness of glass ionomer/fluorinated graphene composite material prepared by the present invention.It can be with See compared to conventional glass-ionomer cement, with the increase of fluorinated graphene additive amount, the microhardness of composite material It is greatly improved.Wherein, the additive amount of fluorinated graphene is that the group of 2wt% has highest microhardness.
Fig. 2 is the compressive strength of glass ionomer/fluorinated graphene composite material prepared by the present invention.It compares In conventional glass-ionomer cement, with the increase of fluorinated graphene additive amount, the compressive strength of composite material is gradually increased. Wherein, the additive amount of fluorinated graphene is that the group of 2wt% has highest compressive strength.
Fig. 3 is the real-time friction coefficient of glass ionomer/fluorinated graphene composite material prepared by the present invention. It can be seen that it is added to the friction coefficient reduction of the glass ionomer composite material of fluorinated graphene, wherein fluorinated graphene Additive amount be 4wt% group have minimum friction coefficient.
Fig. 4 is the wear rate of glass ionomer/fluorinated graphene composite material prepared by the present invention.It can see It is gradually reduced to the wear rate with the increase of fluorinated graphene additive amount, composite material.
Fig. 5 is the bacteriostasis rate of glass ionomer/fluorinated graphene composite material prepared by the present invention.It can see It arrives, the addition of fluorinated graphene enhances the biocidal property of conventional glass-ionomer cement, and with the increase of additive amount, multiple The biocidal property of condensation material enhances therewith.
Specific embodiment
Embodiment 1:
(1) fluorinated graphene is prepared:The graphene oxide that 100mg is prepared according to Hummers methods(Graphene oxide)It adds in In 80mL ultra-pure waters, ultrasonic 30min uniformly disperses graphene oxide, is centrifuged off insoluble substance, which is transferred to In the stainless steel autoclave of 100 mL Teflon linings, 10 mL concentrated nitric acids and 10mL40% hydrofluoric acid are sequentially added under stiring Solution.Sealing autoclave, 180 DEG C of heating 12h, it is to be fluorinated that the 80 DEG C of oil baths of gained clear solution, which are evaporated to obtain white powder, Graphene.
(2) fluorinated graphene prepared in 20mg steps (1) is taken, adds in 10 mL absolute ethyl alcohol ultrasonic disperses 30min.It will 1980mg glass ionomer pulvis is added in the dispersion solution of the absolute ethyl alcohol of fluorinated graphene, and mixed solution is surpassed Glass ionomer and fluorinated graphene dispersion solution are obtained after sound, it in mortar is ground uniformly, is evaporated completely ethyl alcohol Entirely, the content for obtaining fluorinated graphene is fluorinated graphene/glass ionomer mixing powder of 1wt%.
(3) fluorinated graphene/glass ionomer mixing powder and liquor prepared step (2) is according to 2:1 ratio Example is adjusted and is mixed, and the question handler phase makes sample.
The made new material performance test of the present embodiment:
Prepared by the sample of standardization, tested under the conditions of artificial saliva, compare the traditional glass of current Clinical practice from Sub- cement, microhardness increase 51.2%, and compression strength increases 46.5%, and friction coefficient reduces 19.4%, wear rate drop Low 52.5%, to the bacteriostasis rate of staphylococcus aureus up to 66.5%, streptococcus mutans are up to 55.7%.
Embodiment 2:
(1) fluorinated graphene is prepared:100mg is added according to graphene oxide prepared by Hummers methods in 80mL ultra-pure waters, Ultrasonic 30min, uniformly disperses graphene oxide, is centrifuged off insoluble substance, which is transferred to 100 mL Teflon In the stainless steel autoclave of lining, 10 mL concentrated nitric acids and 10mL40% HF solution are sequentially added under stiring.Sealing autoclave, 180 DEG C of heating 12h, it is fluorinated graphene that the 80 DEG C of oil baths of gained clear solution, which are evaporated to obtain white powder,.
(2) fluorinated graphene prepared in 40mg steps (1) is taken, adds in 10 mL absolute ethyl alcohol ultrasonic disperse 30min, with 1960mg pulvis is added in the dispersion solution of the absolute ethyl alcohol of fluorinated graphene, will obtain glass ion after mixed solution ultrasound Cement and fluorinated graphene dispersion solution, it is ground uniformly in mortar, is made ethyl alcohol volatilization complete, is obtained fluorinated graphene Content be 2wt% fluorinated graphene/glass ionomer mixing powder.
(3) fluorinated graphene/glass ionomer mixing powder and liquor prepared step (2) is according to 2:1 ratio Example is adjusted and is mixed, and the question handler phase makes sample.
The made new material performance test of the present embodiment:
Prepared by the sample of standardization, tested under the conditions of artificial saliva, compare the traditional glass of current Clinical practice from Sub- cement, microhardness increase 53.7%, and compression strength increases 59.5%, and friction coefficient reduces 20.6%, wear rate drop Low 61.1%, to the bacteriostasis rate of staphylococcus aureus up to 75.9%, streptococcus mutans are up to 69.3%.
Table 1 is the microhardness of different fluorinated graphene content groups materials, compressive strength and bending strength value.

Claims (2)

1. a kind of novel mouth section glass ionomer/fluorinated graphene composite material, it is characterised in that the composite material leads to Following methods are crossed to be prepared:
1)Fluorinated graphene powder is added in the dispersion solution of the ultrasonic absolute ethyl alcohol for obtaining fluorinated graphene in absolute ethyl alcohol;
2)By glass ionomer pulvis add in fluorinated graphene absolute ethyl alcohol dispersion solution in, ultrasound obtain glass from Sub- cement and fluorinated graphene dispersion solution, it grinds in mortar uniformly, after making ethyl alcohol volatilization complete, obtain glass from Sub- cement and fluorinated graphene mixing powder;
3)Mixing powder and glass ionomer liquor tune are mixed, novel artificial tooth packing material is obtained after its curing.
2. composite material as described in claim 1, it is characterised in that the mixing powder and glass ionomer liquor Mass ratio is 2:1.
CN201711390207.4A 2017-12-21 2017-12-21 A kind of novel mouth section glass ionomer/fluorinated graphene composite material Pending CN108245433A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109331220A (en) * 2018-10-22 2019-02-15 张小伏 A kind of preparation method of orthopaedics bone cement/fluorinated graphene composite material
CN110252030A (en) * 2019-05-30 2019-09-20 辽宁兰晶科技有限公司 A kind of preparation method and application of quantum graphene automobile filter filter material
CN112043607A (en) * 2020-08-12 2020-12-08 华南理工大学 Glass ion cement/straight-chain polyurea-amine modified inorganic fiber composite material for stomatology department
CN113116732A (en) * 2021-03-19 2021-07-16 兰州大学 Novel high-strength antibacterial glass cement composite material containing guanidine component for stomatology department

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1679466A (en) * 2005-02-01 2005-10-12 中国科学院长春应用化学研究所 Liquid of light curing glass ion cement and preparation thereof
CN102174141A (en) * 2011-03-21 2011-09-07 北京化工大学 Method for preparing glass ionomer cement liquid with low dissolubility and acidity
CN105967175A (en) * 2016-05-16 2016-09-28 河南工业大学 Preparation method of water-soluble fluorinated graphene
CN106511102A (en) * 2016-11-03 2017-03-22 中国科学院兰州化学物理研究所 Novel oral denture material and preparation method thereof
CN107213022A (en) * 2017-06-09 2017-09-29 武汉理工大学 A kind of preprocess method of glass ionomer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1679466A (en) * 2005-02-01 2005-10-12 中国科学院长春应用化学研究所 Liquid of light curing glass ion cement and preparation thereof
CN102174141A (en) * 2011-03-21 2011-09-07 北京化工大学 Method for preparing glass ionomer cement liquid with low dissolubility and acidity
CN105967175A (en) * 2016-05-16 2016-09-28 河南工业大学 Preparation method of water-soluble fluorinated graphene
CN106511102A (en) * 2016-11-03 2017-03-22 中国科学院兰州化学物理研究所 Novel oral denture material and preparation method thereof
CN107213022A (en) * 2017-06-09 2017-09-29 武汉理工大学 A kind of preprocess method of glass ionomer

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109331220A (en) * 2018-10-22 2019-02-15 张小伏 A kind of preparation method of orthopaedics bone cement/fluorinated graphene composite material
CN110252030A (en) * 2019-05-30 2019-09-20 辽宁兰晶科技有限公司 A kind of preparation method and application of quantum graphene automobile filter filter material
CN112043607A (en) * 2020-08-12 2020-12-08 华南理工大学 Glass ion cement/straight-chain polyurea-amine modified inorganic fiber composite material for stomatology department
CN112043607B (en) * 2020-08-12 2023-04-21 华南理工大学 Glass ion water portal/linear polyurea-amine modified inorganic fiber composite material for stomatology
CN113116732A (en) * 2021-03-19 2021-07-16 兰州大学 Novel high-strength antibacterial glass cement composite material containing guanidine component for stomatology department
CN113116732B (en) * 2021-03-19 2023-12-22 兰州大学 Antibacterial glass water-gate composite material containing guanidine component in stomatology

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Application publication date: 20180706

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