CN106726627A - Seamless tooth filling material and its preparation technology - Google Patents
Seamless tooth filling material and its preparation technology Download PDFInfo
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- CN106726627A CN106726627A CN201611127073.2A CN201611127073A CN106726627A CN 106726627 A CN106726627 A CN 106726627A CN 201611127073 A CN201611127073 A CN 201611127073A CN 106726627 A CN106726627 A CN 106726627A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/898—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/813—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising iron oxide
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/816—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising titanium oxide
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/891—Compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses seamless tooth filling material and its preparation technology, the tooth filling material is obtained as prepared by following raw material, in parts by weight for：14 28 parts of fluorinated acrylic ester, 5 13 parts of amine modified epoxy acrylic ester, 3 10 parts of bisphenol-A propyl-dimethyl acrylate, 49 parts of cystine diethylester, 16 parts of 3 chlorine, 2 hydroxypropyl-trimethyl ammonium chloride, 0.8 3.6 parts of eucalyptol, 2.2 5 parts of Nano filling, 36 parts of hyaluronic acid magnesium, 1.8 4 parts of polyvinyl alcohol, 2.6 5 parts of Boratex, 0.5 2 parts of camphorsulfonic acid ester, 0.2 1.1 parts of p methoxy phenol, 1.4 3 parts of boron trifluoride monoethanolamine, 0.1 1.2 parts of silane coupler.The abrasivity of the tooth filling material prepared by the present invention is significantly improved, and shrinkage factor reduction, mechanical strength is high high with tooth adhesion strength, and service life was up to more than 20 years.
Description
Technical field
The invention belongs to biology medical material technical field, and in particular to seamless tooth filling material and its preparation work
Skill.
Background technology
With the change of diet structure and eating habit, mouth disease particularly tooth dental caries incidence constantly rises.Carious tooth
It is that hard tooth tissue caused by many factors compound action in oral cavity carries out lesions, shows as inanimate matter demineralization and organic
Matter is decomposed, with disease from color change to the evolution process for forming substantive lesions；And carious tooth is bacteriosis,
It can trigger pulpitis and periapical inflammation, or even can cause alveolar bone and inflammation of jaws, serious harm human health.With medical science
The improvement of the deep and technology of research, cavity recovery technique is carried out clinically using increasingly using Dental Erosion packing material
Extensively.
At present, clinically conventional tooth filling material has metal material, ceramic material, glass material, compound resin material
Material etc., wherein compound resin tooth packing material is because its color and luster is close to tooth, and specious and clinical manipulation is simple and standby
Liked by many patients.But there is shrinkage factor when solidifying and cause gap greatly and cause tooth to fill out in compound resin tooth packing material
Fill coming off or producing secondary cavity for material, and the easily defect such as allergy, resistance to compression, wearability and poor heat resistance.Although research
Scholar is attempted with some method of modifying, and the monomer for example with macromolecule reduces contraction, and adds wear resistant filler to improve
Wearability etc., but its modified effect is not ideal enough.
The content of the invention
It is an object of the invention to provide seamless tooth filling material and its preparation technology, to solve above-mentioned at least one skill
Art problem.
Technical scheme is come as follows：
Seamless tooth filling material, obtains as prepared by following raw material, in parts by weight for：Fluorinated acrylic ester 14-28 parts,
5-13 parts of amine modified epoxy acrylic ester, bisphenol-A -3-10 parts of propyl-dimethyl acrylate, 4-9 parts of cystine diethylester, 3-
Chloro-2-hydroxypropyl-trimethyl ammonium chloride 1-6 parts, eucalyptol 0.8-3.6 parts, Nano filling 2.2-5 parts, 3-6 parts of hyaluronic acid magnesium,
Polyvinyl alcohol 1.8-4 parts, Boratex 2.6-5 parts, 0.5-2 parts of camphorsulfonic acid ester, p methoxy phenol 0.2-1.1 parts, it is borontrifluoride
1.4-3 parts, silane coupler 0.1-1.2 parts of boron monoethanolamine；
The Nano filling is that mass ratio is 1:（0.2-0.6）:（0.1-0.4）:（0.5-0.9）Halloysite nanotubes powder,
Nano silica fume, zinc oxide, the mixture of fluorination ytterbium；The specific surface area of the halloysite nanotubes is 53.6 m2/g.
In above-mentioned technical proposal, element composition and its mass fraction in the halloysite nanotubes are：Al2O3 34-40
wt.%、BaO 0.8-1.2 wt.%、TiO2 0.02-0.05wt.%、Fe2O30.3-1 wt.%, balance of SiO2。
In above-mentioned technical proposal, the Nano filling is that mass ratio is 1:0.28:0.13:0.74 halloysite nanotubes powder
End, nano silica fume, zinc oxide, the mixture of fluorination ytterbium.
In above-mentioned technical proposal, obtained as prepared by following raw material, in parts by weight for：Fluorinated acrylic ester 16-25 parts,
5.8-11 parts of amine modified epoxy acrylic ester, bisphenol-A -3.5-9.2 parts of propyl-dimethyl acrylate, cystine diethylester 4.5-
8 parts, 1.6-5.2 parts of 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, eucalyptol 1.1-3.2 parts, Nano filling 2.5-4.7 parts, it is transparent
Matter acid 3.7-5.4 parts of magnesium, polyvinyl alcohol 2.1-3.8 parts, Boratex 2.8-4.6 parts, 0.7-1.6 parts of camphorsulfonic acid ester, to methoxy
0.4-1 parts of base phenol, 1.6-2.3 parts, silane coupler 0.2-1 parts of boron trifluoride monoethanolamine.
In above-mentioned technical proposal, the silane coupler is γ aminopropyltriethoxy silane, γ-glycidol ether
Oxygen oxypropyl trimethyl silane or γ-methacryloxypropyl trimethoxy silane.
Another technical scheme of the invention is come as follows：
The preparation technology of seamless tooth filling material, including following preparation process：
（1）Weigh by weight；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 30-50min is stirred,
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 50-70 DEG C, stir 30-80min；Be subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides,
Hyaluronic acid magnesium and Boratex, continuation stir 20-50min at 50-70 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 12-24 hours at 25-40 DEG C, obtained final product
Seamless tooth filling material.
Further, the preparation technology of seamless tooth filling material, including following preparation process：
（1）Weigh by weight；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 45min is stirred, then
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 68 DEG C, stir 40min；It is subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, hyalomitome
Sour magnesium and Boratex, continuation stir 35min at 55 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 18 hours at 30 DEG C, obtained final product seamless
Tooth filling material.
As a result of above technical scheme, beneficial effects of the present invention are：
The abrasivity of the tooth filling material prepared by the present invention is significantly improved, its friction 150,000 times after thickness decrement be only
1.8um and following, shrinkage factor is reduced to 1.57-1.74%, while mechanical strength is high, its compressive strength is higher than 360MPa, and bending resistance is strong
Degree is higher than 150MPa, and the tooth filling material is high with tooth adhesion strength in addition, and service life was up to more than 20 years.
Specific embodiment
With reference to embodiment, the present invention is described in further detail.Following examples are not used to illustrate the present invention, but not
For limiting the scope of the present invention.
Embodiment 1
Seamless tooth filling material, obtains as prepared by following raw material, in parts by weight for：14 parts of fluorinated acrylic ester, amine
5 parts of modified epoxy acrylic ester, bisphenol-A -3 parts of propyl-dimethyl acrylate, 4 parts of cystine diethylester, the chloro- 2- hydroxypropyls of 3-
1 part of trimethyl ammonium chloride, 0.8 part of eucalyptol, 2.2 parts of Nano filling, 3 parts of hyaluronic acid magnesium, 1.8 parts of polyvinyl alcohol, Boratex
2.6 parts, 0.5 part of camphorsulfonic acid ester, 0.2 part of p methoxy phenol, 1.4 parts of boron trifluoride monoethanolamine, silane coupler 0.1；
Wherein, the Nano filling is that mass ratio is 1:0.2:0.1:0.5 halloysite nanotubes powder, nano silica fume, oxidation
The mixture of zinc, fluorination ytterbium；The specific surface area of the halloysite nanotubes is 53.6 m2/g.In the halloysite nanotubes
Element is constituted and its mass fraction is：Al2O3 34 wt.%、BaO 0.8 wt.%、TiO2 0.02wt.%、Fe2O30.3 wt.%,
Balance of SiO2.The Nano filling is that mass ratio is 1:0.28:0.13:0.74 halloysite nanotubes powder, nano silica fume,
The mixture of zinc oxide, fluorination ytterbium.The silane coupler is γ aminopropyltriethoxy silane.
The preparation technology of seamless tooth filling material, including following preparation process：
（1）Weighed by above-mentioned weight portion；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 30min is stirred, then
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 50 DEG C, stir 30min；It is subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, hyalomitome
Sour magnesium and Boratex, continuation stir 20min at 50 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 12-24 hours at 25 DEG C, obtain final product nothing
Gap tooth filling material.
Embodiment 2
Seamless tooth filling material, obtains as prepared by following raw material, in parts by weight for：28 parts of fluorinated acrylic ester, amine
13 parts of modified epoxy acrylic ester, bisphenol-A -10 parts of propyl-dimethyl acrylate, 9 parts of cystine diethylester, the chloro- 2- hydroxypropyls of 3-
6 parts of base trimethyl ammonium chloride, 3.6 parts of eucalyptol, 5 parts of Nano filling, 6 parts of hyaluronic acid magnesium, polyvinyl alcohol 1.8-4 parts, boric acid
5 parts of sodium, 2 parts of camphorsulfonic acid ester, 1.1 parts of p methoxy phenol, 3 parts of boron trifluoride monoethanolamine, 1.2 parts of silane coupler；
Wherein, the Nano filling is that mass ratio is 1:0.6:0.4:0.9 halloysite nanotubes powder, nano silica fume, oxidation
The mixture of zinc, fluorination ytterbium；The specific surface area of the halloysite nanotubes is 53.6 m2/g.In the halloysite nanotubes
Element is constituted and its mass fraction is：Al2O3 40 wt.%、BaO 1.2 wt.%、TiO2 0.05wt.%、Fe2O31 wt.%, it is remaining
It is SiO to measure2.The Nano filling is that mass ratio is 1:0.28:0.13:0.74 halloysite nanotubes powder, nano silica fume, oxygen
Change zinc, the mixture of fluorination ytterbium.The silane coupler is γ-glycidyl ether oxygen propyl trimethyl silane.
The preparation technology of seamless tooth filling material, including following preparation process：
（1）Weighed by above-mentioned weight portion；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 30-50min is stirred,
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 50-70 DEG C, stir 30-80min；Be subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides,
Hyaluronic acid magnesium and Boratex, continuation stir 20-50min at 50-70 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 12-24 hours at 25-40 DEG C, obtained final product
Seamless tooth filling material.
Embodiment 3
Seamless tooth filling material, obtains as prepared by following raw material, in parts by weight for：16 parts of fluorinated acrylic ester, amine
5.8 parts of modified epoxy acrylic ester, bisphenol-A -3.5 parts of propyl-dimethyl acrylate, 4.5 parts of cystine diethylester, the chloro- 2- of 3-
1.6 parts of hydroxypropyl-trimethyl ammonium chloride, 1.1 parts of eucalyptol, 2.5 parts of Nano filling, 3.7 parts of hyaluronic acid magnesium, polyvinyl alcohol 2.1
It is part, 2.8 parts of Boratex, 0.7 part of camphorsulfonic acid ester, 0.4 part of p methoxy phenol, 1.6 parts of boron trifluoride monoethanolamine, silane coupled
0.2 part of agent；
Wherein, the Nano filling is that mass ratio is 1:0.3:0.15:0.7 halloysite nanotubes powder, nano silica fume, oxidation
The mixture of zinc, fluorination ytterbium；The specific surface area of the halloysite nanotubes is 53.6 m2/g.In the halloysite nanotubes
Element is constituted and its mass fraction is：Al2O3 37 wt.%、BaO 1.1 wt.%、TiO2 0.04wt.%、Fe2O30.7 wt.%,
Balance of SiO2.The Nano filling is that mass ratio is 1:0.28:0.13:0.74 halloysite nanotubes powder, nano silica fume,
The mixture of zinc oxide, fluorination ytterbium.The silane coupler is γ-methacryloxypropyl trimethoxy silane.
The preparation technology of seamless tooth filling material, including following preparation process：
（1）Weighed by above-mentioned weight portion；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 45min is stirred, then
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 68 DEG C, stir 55min；It is subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, hyalomitome
Sour magnesium and Boratex, continuation stir 45min at 60 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 18 hours at 38 DEG C, obtained final product seamless
Tooth filling material.
Embodiment 4
Seamless tooth filling material, obtains as prepared by following raw material, in parts by weight for：25 parts of fluorinated acrylic ester, amine
11 parts of modified epoxy acrylic ester, bisphenol-A -9.2 parts of propyl-dimethyl acrylate, 8 parts of cystine diethylester, the chloro- 2- hydroxyls of 3-
5.2 parts of hydroxypropyltrimonium chloride, 3.2 parts of eucalyptol, 4.7 parts of Nano filling, 5.4 parts of hyaluronic acid magnesium, polyvinyl alcohol 3.8
Part, 4.6 parts of Boratex, 1.6 parts of camphorsulfonic acid ester, 1 part of p methoxy phenol, 2.3 parts of boron trifluoride monoethanolamine, silane coupler
1 part；
Wherein, the Nano filling is that mass ratio is 1:0.35:0.2:0.6 halloysite nanotubes powder, nano silica fume, oxidation
The mixture of zinc, fluorination ytterbium；The specific surface area of the halloysite nanotubes is 53.6 m2/g.In the halloysite nanotubes
Element is constituted and its mass fraction is：Al2O3 37 wt.%、BaO 0.9 wt.%、TiO2 0.02-0.05wt.%、Fe2O3 0.5
Wt.%, balance of SiO2.The Nano filling is that mass ratio is 1:0.28:0.13:0.74 halloysite nanotubes powder, nanometer
Silica flour, zinc oxide, the mixture of fluorination ytterbium.The silane coupler is γ aminopropyltriethoxy silane.
The preparation technology of seamless tooth filling material, including following preparation process：
（1）Weighed by above-mentioned weight portion；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 45min is stirred, then
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 68 DEG C, stir 40min；It is subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, hyalomitome
Sour magnesium and Boratex, continuation stir 35min at 55 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 18 hours at 30 DEG C, obtained final product seamless
Tooth filling material.
Comparative example 1
It is in place of this comparative example and the difference of embodiment 1：Without bisphenol-A-propyl-dimethyl acrylate, Boratex and volatile oil extracted from eucalyptus' leaves or twigs
Essence.Other components, content of this comparative example and preparation method thereof are with embodiment 2.
Comparative example 2
It is in place of this comparative example and the difference of embodiment 1：Without 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides and boron trifluoride second
Hydramine.Other components, content of this comparative example and preparation method thereof are with embodiment 2.
Comparative example 3
It is in place of this comparative example and the difference of embodiment 1：The Nano filling is nano silica fume.The other components of this comparative example,
Content and preparation method thereof is with embodiment 2.
Performance test
Correlated performance test is carried out to the tooth filling material prepared by above-described embodiment and comparative example, its test result see the table below
It is shown：
| Compressive strength/MPa | Bending strength/MPa | Abrasion/um（Rub thickness decrement after 150,000 times） | Polymerization shrinkage/% | |
| Embodiment 1 | 365 | 158 | 1.8 | 1.74 |
| Embodiment 2 | 372 | 164 | 1.3 | 1.68 |
| Embodiment 3 | 381 | 172 | 1.1 | 1.63 |
| Embodiment 4 | 376 | 168 | 1.2 | 1.57 |
| Comparative example 1 | 322 | 116 | 2.2 | 1.87 |
| Comparative example 2 | 341 | 124 | 2.1 | 1.92 |
| Comparative example 3 | 253 | 106 | 2.7 | 2.53 |
After tested, the abrasivity of tooth filling material prepared by the present invention is significantly improved, and thickness subtracts after its friction 150,000 times
Amount is only 1.8um and following, and shrinkage factor is reduced to 1.57-1.74%, while mechanical strength is high, its compressive strength is higher than 360MPa,
Bending strength is higher than 150MPa, and the tooth filling material is high with tooth adhesion strength in addition, and service life was up to more than 20 years.
Claims (7)
1. seamless tooth filling material, it is characterised in that obtained as prepared by following raw material, in parts by weight for：Fluorination third
14-28 parts of olefin(e) acid ester, 5-13 parts of amine modified epoxy acrylic ester, bisphenol-A -3-10 parts of propyl-dimethyl acrylate, cystine
Diethylester 4-9 parts, 1-6 parts of 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, eucalyptol 0.8-3.6 parts, Nano filling 2.2-5 parts, thoroughly
3-6 parts of magnesium of bright matter acid, polyvinyl alcohol 1.8-4 parts, Boratex 2.6-5 parts, 0.5-2 parts of camphorsulfonic acid ester, p methoxy phenol
0.2-1.1 parts, 1.4-3 parts, silane coupler 0.1-1.2 parts of boron trifluoride monoethanolamine；
The Nano filling is that mass ratio is 1:（0.2-0.6）:（0.1-0.4）:（0.5-0.9）Halloysite nanotubes powder,
Nano silica fume, zinc oxide, the mixture of fluorination ytterbium；The specific surface area of the halloysite nanotubes is 53.6 m2/g。
2. seamless tooth filling material according to claim 1, it is characterised in that in the halloysite nanotubes
Element is constituted and its mass fraction is：Al2O3 34-40 wt.%、BaO 0.8-1.2 wt.%、TiO2 0.02-0.05wt.%、
Fe2O30.3-1 wt.%, balance of SiO2。
3. seamless tooth filling material according to claim 1, it is characterised in that the Nano filling is for mass ratio
1:0.28:0.13:0.74 halloysite nanotubes powder, nano silica fume, zinc oxide, the mixture of fluorination ytterbium.
4. seamless tooth filling material according to claim 1, it is characterised in that obtained as prepared by following raw material,
It is in parts by weight：Fluorinated acrylic ester 16-25 parts, 5.8-11 parts of amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl
Acrylate 3.5-9.2 parts, 4.5-8 parts of cystine diethylester, 1.6-5.2 parts of 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, volatile oil extracted from eucalyptus' leaves or twigs
It is smart 1.1-3.2 parts, Nano filling 2.5-4.7 parts, 3.7-5.4 parts of hyaluronic acid magnesium, polyvinyl alcohol 2.1-3.8 parts, Boratex
2.8-4.6 parts, 0.7-1.6 parts of camphorsulfonic acid ester, p methoxy phenol 0.4-1 parts, 1.6-2.3 parts of boron trifluoride monoethanolamine, silicon
0.2-1 parts of alkane coupling agent.
5. seamless tooth filling material according to claim 1, it is characterised in that the silane coupler is γ-ammonia
Base propyl-triethoxysilicane, γ-glycidyl ether oxygen propyl trimethyl silane or γ-methacryloxypropyl trimethoxy
Base silane.
6. the preparation technology of the seamless tooth filling material according to claim 1-5 any one, it is characterised in that bag
Include following preparation process：
（1）Weigh by weight；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 30-50min is stirred,
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 50-70 DEG C, stir 30-80min；Be subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides,
Hyaluronic acid magnesium and Boratex, continuation stir 20-50min at 50-70 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 12-24 hours at 25-40 DEG C, obtained final product
Seamless tooth filling material.
7. the preparation technology of seamless tooth filling material according to claim 6, it is characterised in that including following preparation
Step：
（1）Weigh by weight；
（2）Silane coupler is made into the ethanol solution of 3wt.%, polyvinyl alcohol and eucalyptol is subsequently adding, 45min is stirred, then
Nano filling is added, is uniformly mixed, freeze-drying obtains modified Nano filling；
（3）By fluorinated acrylic ester, amine modified epoxy acrylic ester, bisphenol-A-propyl-dimethyl acrylate, cystine diethyl
Ester and p methoxy phenol are heated to 68 DEG C, stir 40min；It is subsequently adding 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, hyalomitome
Sour magnesium and Boratex, continuation stir 35min at 55 DEG C, obtain resin compound；
（4）By step（2）In modified Nano filling add to step（3）In resin compound, be thoroughly mixed it is uniform,
Camphorsulfonic acid ester and boron trifluoride monoethanolamine are subsequently adding, are stirred, be vacuum dried 18 hours at 30 DEG C, obtained final product seamless
Tooth filling material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108542792A (en) * | 2018-04-25 | 2018-09-18 | 佛山科学技术学院 | A kind of antibacterial dental filling packing material |
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| CN103622835A (en) * | 2013-12-02 | 2014-03-12 | 天津大学 | DMC-MMA (methyl methacrylate)-halloysite copolymerized denture base material and preparation method thereof |
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| CN105853241A (en) * | 2016-06-21 | 2016-08-17 | 林春梅 | Dental adhesive and preparation method thereof |
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| CN103040631A (en) * | 2013-01-23 | 2013-04-17 | 常州南京大学高新技术研究院 | Antibacterial type inorganic whisker functional composite as well as preparation method and application thereof |
| CN103622835A (en) * | 2013-12-02 | 2014-03-12 | 天津大学 | DMC-MMA (methyl methacrylate)-halloysite copolymerized denture base material and preparation method thereof |
| CN105193634A (en) * | 2015-09-21 | 2015-12-30 | 江苏科技大学 | Dental restoration filling material containing special function monomer and preparation method of dental restoration filling material |
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