CN100431517C - Method for preparing fiber reinforced composite material used for artificial tooth base - Google Patents
Method for preparing fiber reinforced composite material used for artificial tooth base Download PDFInfo
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- CN100431517C CN100431517C CNB2006101050215A CN200610105021A CN100431517C CN 100431517 C CN100431517 C CN 100431517C CN B2006101050215 A CNB2006101050215 A CN B2006101050215A CN 200610105021 A CN200610105021 A CN 200610105021A CN 100431517 C CN100431517 C CN 100431517C
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- zirconium oxide
- oxide fibre
- acrylic acid
- methyl ester
- acid methyl
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Abstract
A fiber reinforced dental material used as the base of artificial tooth is prepared from zirconium oxide fibers through immersing in H2O2, baking, mixing with distilled water, sequentially adding sodium lauryl benzosulfonate, tributyl phosphate and polyvinyl alcohol, adding the mixture of benzoyl peroxide, methyl methylacrylate and methyl acrylate, suspended polymerizing reaction, and moulding.
Description
Technical field
The present invention relates to a kind of preparation method of dental materials, particularly a kind of preparation method of fiber reinforced composite material used for artificial tooth base.
Background technology
China has stepped into aging society, and the ratio of crowd's dens in dente tooth disappearance of growing up constantly increases, and wears the requirement that a secondary robust artificial tooth has become more and more people.Base is as one of three big important documents of removable denture, and research in decades mainly concentrates on a series of materials such as polymethyl methacrylate base holder, cochrome casting frame base, pure titanium casting support base.Tradition is used as the biomaterial of dental prosthetic, comprises materials such as metal, pottery, macromolecule, has many shortcomings that are difficult to overcome, and can not satisfy the demand as the metal material aesthetic property; Ceramic material fragility is big, easily bursts apart; Macromolecular material is low not wear-resisting because of its hardness.And compound these materials, form composite biological material, then in Oral Repair, have more widely and use.
Polymer matrix composites have specific strength and specific stiffness height, designability is strong, the fatigue crack-resistant performance is good, corrosion-resistant, physical dimension good stability and be convenient to the integrally formed distinct advantages of large tracts of land, also have special electromagnetic performance and wave-absorbing and camouflage effect, demonstrated fully structure set carrying and function distinguishing feature.Be widely used in fields such as Aero-Space, stationery sports goods, textile machine, medical apparatus and instruments, biological engineering, construction material, chemical machinery, haulage vehicle.The German at first proposed to use the heat curing-type methyl methacrylate to substitute the vulcanite that generally adopted at that time in 1936, made denture base material, and the quality of artificial tooth has obtained significant raising.Because polymethyl methacrylate is simple to operate, biocompatibility is good, and is with low cost, by wide clinical application, is the main material of making basal seat area at present in recent years.But it has easily burn gingiva and oral cavity mucous membrane tissue, and color is single, easy to change in the use, and shortcoming such as during indirect production costs.Especially for a long time the fracture of basal seat area, especially easy to crack always the failing of the total basal seat area of the upper jaw is well solved.This be since the mechanical performance of polymethyl methacrylate relatively poor due to.
Effectively way is that fiber or some nano inorganic materials that Aramid (Kevlar), glass, aramid fiber, ultra-high molecular weight polyethylene, heat reactive resin are made are added base respectively at present, to improve its mechanical strength.But the Aramid fiber makes base present yellow respectively, and is exposed to base when surface and is difficult for polishing; Heat reactive resin fiber and heat reactive resin base are bonding, but operation inconvenience, so the heat reactive resin fiber seldom uses; Superhigh molecular weight polyethylene fibers and heat reactive resin bad adhesion need surface treatment.Glass fibre is attractive in appearance, studies morely at present, but that the shortcoming of its maximum is hardness is too low.Xu Dongxuan etc. add the fractional super strong polyethylene fiber of different quality in artificial tooth base resin, test its flexural strength, find the flexural strength of the denture base resin of adding super strong polyethylene fiber, when 3.5wt%, increase by 30.5%, reach maximum [Xu Dongxuan, Cheng Xiangrong, Zhang Yufeng, super strong polyethylene fiber strengthens resin base Performance Experiment, stomatology research, 2003,19 (4): 272-273].Zhang Lianyun finds to add the etched glass fibre of non-directional epoxy silane electronics in chemosetting type acrylic resin, can make the hot strength of resin and the elastic modelling quantity [Zhang Lianyun that has significant improvement, the applied research of removable denture surface treatment new material, modern stomatology magazine, 1999,13 (2): 99～100]].Human glass fiber reinforced polyester methyl methacrylate/hydroxyapatite composite materials such as Wan Tao, respond well [Chen Bo waits .PMMA/HA-GF composite [J] for ten thousand great waves, Yan Yuhua. China YouSe Acta Metallurgica Sinica, 2002,12 (5): 935-939].Yu Sheng etc. utilize the method for in-situ polymerization will study nanometer SiO
2Granule is toughness reinforcing to the enhancing of polymethyl methacrylate (PMMA) base.Discovery adds certain density nanometer SiO in polymethyl methacrylate (PMMA) base
2Granule can improve the bending strength and the hot strength of traditional basal seat area, is expected to solve that its fragility is big, frangibility, [Yu Sheng, Xu Lian comes aged problem, Li Changfu, nanometer (PMMA/SiO
2) basic research of basal seat area composite, Medical University Of Tianjin's journal, 2003,9 (1): 90-92].
Zirconium dioxide is unique metal-oxide with acidity, alkalescence, oxidisability and reproducibility, and there is bigger using value aspects such as therefore synthetic in industry, catalyst, catalyst carrier, special cermacis.Zirconium oxide fibre is as high-temperature insulation and ceramic-ceramic composite.The stabilized zirconia pottery has certain application because of its high-toughness high-strength in Oral Repair, as being used as a stake nuclear material, interior hat and mounting system (the aluminum porcelain of Zirconium oxide plasticizing, machinable zirconia ceramics) etc.Li Shibao etc. infiltrate through pre-polymethyl methacrylate in the porous network structure zirconium oxide, in-situ polymerization, prepare polymethyl methacrylate-zirconium oxide composite organic-inorganic material, bending strength, fracture toughness are significantly improved, this composite can disposablely be prepared dental prosthesis through dental CAD/CAM system machining.ZrO such as [Li Shibao, Chen Chaohui, Wang Zhongyi, the preparation of polymethyl methacrylate-zirconium oxide composite material, National University of Defense technology's journal, 2005,27 (4): 32-36] Sheng Xiangjun
2Strengthen toughness reinforcing dental case, ZrO
2The surface modification dental case, the full porcelain tooth dummy of ZrO2.[Sheng Xiangjun, Jin Zhihao, Wang Yonglan, zirconium oxide are used for the progress that tooth is repaired, silicate circular, 2003, (5): 74-78].Rong Tianjun etc. force down warm liquid-phase sintering with stable tetragonal zirconia polycrystal powder body and sintering aids such as cerium oxide through nothing, can improve the index [Rong Tianjun such as machinability, bending strength, fracture toughness of material; Wang Shiwei, Cheap machinable zirconium oxide ceramic dental repairing body and preparation method thereof, number of patent application: 200510027284.4].
Summary of the invention
The object of the present invention is to provide a kind of preparation method of fiber reinforced composite material used for artificial tooth base, the composite that obtains according to preparation method of the present invention has higher rupture strength and bending modulus, better biocompatibility and chemical stability are a kind of comparatively ideal dental materials.
For achieving the above object, the technical solution used in the present invention is: at first be that 30% hydrogen peroxide soaked 30～60 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate, that acrylic acid methyl ester. is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=8-15ml: 1ml: 0.09-0.48g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 350-450ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.04%-0.06% then, the tributyl phosphate that adds liquid quality 0.05%-0.2% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.06%-0.065% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=0.75%-2.5% adds mixed liquor in fiber dispersion, stir, and is warmed up to 70～90 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 30～50 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 35-45 ℃, vacuum is solidified 8-10h down for the 0.09MPa environment, at room temperature leave standstill 24h, at 85-95 ℃, vacuum is ripening 2-3h under the 0.09MPa environment, promptly can obtain needed product then.
Because the present invention is a raw material with acrylic acid methyl ester., methyl methacrylate, Zirconium oxide fibre, adopt the method for suspension polymerisation, synthesized the zirconium oxide short fiber and strengthened the basic basal seat area composite of polymethyl methacrylate-acrylic acid methyl ester. (PMMA-PMA), synthetic composite have higher rupture strength and a bending modulus.The composite rupture strength is 28.5-52.1MPa, and bending modulus reaches 180-265MPa, and the rupture strength of material and toughness are all than single polymethyl methacrylate and polymethyl acrylate height; And prepared composite fiber is uniformly dispersed, and fiber combines well with basal body interface, is a kind of comparatively ideal dental material.
The specific embodiment
Embodiment 1: at first be that 30% hydrogen peroxide soaked 30 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate (MMA), that acrylic acid methyl ester. (MA) is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=8ml: 1ml: 0.09g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 350ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.04% then, the tributyl phosphate that adds liquid quality 0.05% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.06% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=0.75% adds mixed liquor in fiber dispersion, stir, and is warmed up to 70 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 30 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 35 ℃, vacuum at room temperature leaves standstill 24h for the 0.09MPa environment solidifies 10h down, and then at 85 ℃, vacuum is ripening 3h under the 0.09MPa environment, promptly can obtain needed product.
Embodiment 2: at first be that 30% hydrogen peroxide soaked 60 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate (MMA), that acrylic acid methyl ester. (MA) is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=15ml: 1ml: 0.48g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 450ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.06% then, the tributyl phosphate that adds liquid quality 0.2% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.065% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=2.5% adds mixed liquor in fiber dispersion, stir, and is warmed up to 90 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 30 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 45 ℃, vacuum at room temperature leaves standstill 24h for the 0.09MPa environment solidifies 8h down, and then at 95 ℃, vacuum is ripening 2h under the 0.09MPa environment, promptly can obtain needed product.
Embodiment 3: at first be that 30% hydrogen peroxide soaked 45 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate (MMA), that acrylic acid methyl ester. (MA) is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=12ml: 1ml: 0.32g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 400ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.05% then, the tributyl phosphate that adds liquid quality 0.1% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.062% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=1.5% adds mixed liquor in fiber dispersion, stir, and is warmed up to 80 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 40 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 40 ℃, vacuum at room temperature leaves standstill 24h for the 0.09MPa environment solidifies 9h down, and then at 90 ℃, vacuum is ripening 2.5h under the 0.09MPa environment, promptly can obtain needed product.
Claims (4)
1, a kind of preparation method of fiber reinforced composite material used for artificial tooth base is characterized in that:
1) at first be that 30% hydrogen peroxide soaked 30～60 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃;
2) then with benzoyl peroxide, methyl methacrylate, that acrylic acid methyl ester. is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=8-15ml: 1ml: 0.09-0.48g is standby;
3) Zirconium oxide fibre after next will soak through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 350-450ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.04%-0.06% then, the tributyl phosphate that adds liquid quality 0.05%-0.2% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.06%-0.065% again stirs and makes fiber dispersion;
4) mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=0.75%-2.5% adds mixed liquor prepared in the step 2 in fiber dispersion, stir, be warmed up to 70～90 ℃ then and carry out suspension polymerisation, react and take out polymer after 30～50 minutes;
5) at last with the polymer immigration die for molding of above-mentioned taking-up, at 35-45 ℃, vacuum is that the 0.09MPa environment solidifies 8-10h down, at room temperature leave standstill 24h, at 85-95 ℃, vacuum is ripening 2-3h under the 0.09MPa environment, promptly can obtain needed product then.
2, the preparation method of fiber reinforced composite material used for artificial tooth base according to claim 1 is characterized in that: at first be that 30% hydrogen peroxide soaked 30 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate, that acrylic acid methyl ester. is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=8ml: 1ml: 0.09g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 350ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.04% then, the tributyl phosphate that adds liquid quality 0.05% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.06% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=0.75% adds mixed liquor in fiber dispersion, stir, and is warmed up to 70 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 30 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 35 ℃, vacuum at room temperature leaves standstill 24h for the 0.09MPa environment solidifies 10h down, and then at 85 ℃, vacuum is ripening 3h under the 0.09MPa environment, promptly can obtain needed product.
3, the preparation method of fiber reinforced composite material used for artificial tooth base according to claim 1 is characterized in that: at first be that 30% hydrogen peroxide soaked 60 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate, that acrylic acid methyl ester. is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=15ml: 1ml: 0.48g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 450ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.06% then, the tributyl phosphate that adds liquid quality 0.2% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.065% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=2.5% adds mixed liquor in fiber dispersion, stir, and is warmed up to 90 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 30 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 45 ℃, vacuum at room temperature leaves standstill 24h for the 0.09MPa environment solidifies 8h down, and then at 95 ℃, vacuum is ripening 2h under the 0.09MPa environment, promptly can obtain needed product.
4, the preparation method of fiber reinforced composite material used for artificial tooth base according to claim 1 is characterized in that: at first be that 30% hydrogen peroxide soaked 45 minutes with the Zirconium oxide fibre mass concentration, the oven dry back is standby down at 100 ℃; Then with benzoyl peroxide, methyl methacrylate, that acrylic acid methyl ester. is made mixed liquor according to the ratio uniform mixing of methyl methacrylate/acrylic acid methyl ester ./benzoyl peroxide=12ml: 1ml: 0.32g is standby; Secondly Zirconium oxide fibre after will soaking through hydrogen peroxide and distilled water are made into liquid according to the ratio of Zirconium oxide fibre/distilled water=1g: 400ml, the dodecylbenzene sodium sulfonate that in this liquid, adds liquid quality 0.05% then, the tributyl phosphate that adds liquid quality 0.1% after the dispersed with stirring again, after treating that fiber dispersion fully, the polyvinyl alcohol that adds liquid quality 0.062% again stirs and makes fiber dispersion; Mass ratio according to Zirconium oxide fibre/(methyl methacrylate+acrylic acid methyl ester .)=1.5% adds mixed liquor in fiber dispersion, stir, and is warmed up to 80 ℃ then and carries out suspension polymerisation, reacts and takes out polymer after 40 minutes; Polymer with above-mentioned taking-up moves into die for molding at last, and at 40 ℃, vacuum at room temperature leaves standstill 24h for the 0.09MPa environment solidifies 9h down, and then at 90 ℃, vacuum is ripening 2.5h under the 0.09MPa environment, promptly can obtain needed product.
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| CN103740019A (en) * | 2013-12-31 | 2014-04-23 | 上海医疗器械股份有限公司 | Anti-aging self-curing denture base resin and production method thereof |
| CN107537061B (en) * | 2016-06-23 | 2019-11-22 | 辽宁爱尔创生物材料有限公司 | A kind of preparation method of dental composite resin material and its product of preparation |
| CN108743405B (en) * | 2018-06-14 | 2021-03-26 | 中国科学院金属研究所 | Zirconia/resin bionic composite material for false tooth and preparation method thereof |
| CN110353839B (en) * | 2019-07-22 | 2021-08-10 | 深圳市康隆医疗科技有限公司 | False tooth base template and processing technology thereof |
| CN115414259B (en) * | 2022-09-30 | 2023-05-23 | 杭州拉瓦生物科技有限公司 | Customized type fixed denture and manufacturing method thereof |
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