CN115919659A - Dental repair material containing ceramic wetting resin and preparation method thereof - Google Patents
Dental repair material containing ceramic wetting resin and preparation method thereof Download PDFInfo
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- CN115919659A CN115919659A CN202211462301.7A CN202211462301A CN115919659A CN 115919659 A CN115919659 A CN 115919659A CN 202211462301 A CN202211462301 A CN 202211462301A CN 115919659 A CN115919659 A CN 115919659A
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- 239000011347 resin Substances 0.000 title claims abstract description 63
- 229920005989 resin Polymers 0.000 title claims abstract description 63
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000009736 wetting Methods 0.000 title claims abstract description 32
- 239000000919 ceramic Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000008439 repair process Effects 0.000 title abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 89
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 13
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 11
- 239000011147 inorganic material Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910052788 barium Inorganic materials 0.000 claims abstract description 10
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010453 quartz Substances 0.000 claims abstract description 6
- 239000005388 borosilicate glass Substances 0.000 claims abstract description 5
- 239000011368 organic material Substances 0.000 claims abstract description 5
- AXFLWPUWMOTLEY-UHFFFAOYSA-N oxosilicon(2+) oxygen(2-) zirconium(4+) Chemical compound [Si+2]=O.[O-2].[Zr+4].[O-2].[O-2] AXFLWPUWMOTLEY-UHFFFAOYSA-N 0.000 claims abstract description 5
- VLRMTUPMULFHBI-UHFFFAOYSA-N [O-2].[Yb+3].[Si+2]=O Chemical compound [O-2].[Yb+3].[Si+2]=O VLRMTUPMULFHBI-UHFFFAOYSA-N 0.000 claims abstract description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N Propionic acid Chemical group CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000113 methacrylic resin Substances 0.000 claims abstract description 3
- 239000004417 polycarbonate Substances 0.000 claims abstract description 3
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 3
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000000945 filler Substances 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 239000012752 auxiliary agent Substances 0.000 claims description 13
- AMFGWXWBFGVCKG-UHFFFAOYSA-N Panavia opaque Chemical compound C1=CC(OCC(O)COC(=O)C(=C)C)=CC=C1C(C)(C)C1=CC=C(OCC(O)COC(=O)C(C)=C)C=C1 AMFGWXWBFGVCKG-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- HWSSEYVMGDIFMH-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOC(=O)C(C)=C HWSSEYVMGDIFMH-UHFFFAOYSA-N 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 5
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 5
- 229930006711 bornane-2,3-dione Natural products 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000004898 kneading Methods 0.000 claims description 4
- VNQXSTWCDUXYEZ-UHFFFAOYSA-N 1,7,7-trimethylbicyclo[2.2.1]heptane-2,3-dione Chemical compound C1CC2(C)C(=O)C(=O)C1C2(C)C VNQXSTWCDUXYEZ-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- MKVYSRNJLWTVIK-UHFFFAOYSA-N ethyl carbamate;2-methylprop-2-enoic acid Chemical compound CCOC(N)=O.CC(=C)C(O)=O.CC(=C)C(O)=O MKVYSRNJLWTVIK-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 2
- MWCLLHOVUTZFKS-UHFFFAOYSA-N Methyl cyanoacrylate Chemical compound COC(=O)C(=C)C#N MWCLLHOVUTZFKS-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 125000002362 bornane-2,3-dione group Chemical group 0.000 claims description 2
- KWKVJEUILVQMRR-UHFFFAOYSA-N decyl 2-cyanoprop-2-enoate Chemical compound CCCCCCCCCCOC(=O)C(=C)C#N KWKVJEUILVQMRR-UHFFFAOYSA-N 0.000 claims description 2
- 239000003085 diluting agent Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- JJJFUHOGVZWXNQ-UHFFFAOYSA-N enbucrilate Chemical compound CCCCOC(=O)C(=C)C#N JJJFUHOGVZWXNQ-UHFFFAOYSA-N 0.000 claims description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- 239000012257 stirred material Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 239000012855 volatile organic compound Substances 0.000 claims description 2
- 239000000080 wetting agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims 1
- 229940075624 ytterbium oxide Drugs 0.000 claims 1
- 239000000805 composite resin Substances 0.000 abstract description 9
- 238000002444 silanisation Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 239000005548 dental material Substances 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- -1 UDMA Chemical compound 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009837 dry grinding Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910003439 heavy metal oxide Inorganic materials 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Dental Preparations (AREA)
Abstract
The invention relates to the technical field of dental materials, in particular to a dental repair material containing porcelain moistening resin and a preparation method thereof. The ceramic wetting resin is a mixture comprising an inorganic material and an organic substance, the inorganic material is one or more of quartz powder, barium glass powder, lanthanum glass powder, borosilicate glass powder, silicon oxide-zirconium oxide composite powder, silicon oxide-ytterbium oxide composite powder, nano silicon oxide powder, nano zirconium oxide powder or titanium oxide powder, and the organic material is one or more of polycarbonate, polyepoxide, polymerized methacrylic resin or a polymer containing propionate groups; the mass fraction of the inorganic material in the ceramic wetting resin is 50-80%. Compared with the traditional material, the ceramic wetting resin is used, so that the silanization process can be omitted, the uniformity of the material is greatly improved, the shrinkage rate of the composite resin is effectively reduced, and the optical and aesthetic effects of the composite resin are improved.
Description
Technical Field
The invention relates to the technical field of dental materials, in particular to a dental repair material containing porcelain moistening resin and a preparation method thereof.
Background
Dental filling resins are intended to replace missing tooth structures and alter tooth color and contour, thereby enhancing aesthetics. Many commercial resin composites are available for various applications, some optimized for aesthetics, while others are designed specifically for areas subject to higher stresses. The dental restorative composition is essentially constituted by a combination of a polymerizable monomer, a filler and a polymerization initiator. In order to provide the capability of approaching to natural teeth, acrylic resin monomers, high-transmittance inorganic glass fillers, visible light photoinitiators and pigments close to the teeth are selected in the prior art. Fillers make up the major part of the volume or weight of the composite. The filler serves to reinforce the resin matrix, provide adequate transparency, and control the volume shrinkage of the composite during polymerization. Fillers are traditionally mostly inorganic powder fillers, usually obtained by grinding minerals such as quartz, glass or sol-gel derived ceramics. Most fillers contain glass powders of heavy metal oxides such as barium or zinc, and thus they can provide radiopaque visualization effects when exposed to X-rays.
However, the surface of the inorganic powder filler needs to be treated in the using process, otherwise, the compatibility with the acrylic resin monomer is poor, the inorganic powder surface treatment generally adopts silanization treatment, the adopted silane coupling agent is a silane coupling agent containing acrylic groups, and the addition content is generally 5% -10%. However, the particle size of the powder is generally smaller than 0.5-2um, so the silanization process has the following difficulties: 1) The specific surface area of the inorganic powder is large, the surface treatment is difficult, the compatibility is difficult to ensure, the particle size of the powder is small, and granulation is needed to form large powder. 2) The error of the silanization treatment process is large, the silanization process needs hydrolysis, high-speed stirring and other processes, a long time is needed, the uniformity of the powder subjected to surface silanization treatment is difficult to ensure, and 3) the adding and mixing processes of the powder and the resin monomer need a relatively long surface wetting process. In view of the above, it is difficult to ensure interfacial compatibility and particle size distribution of silanized powder, and the following defects are often present: 1) The shrinkage rate of the composite resin is difficult to compensate, and the resin can be broken at any time due to a large shrinkage gap; 2) The optical and aesthetic effects of the composite resin are difficult to ensure; 3) The mechanical strength of the composite resin is difficult to ensure.
Disclosure of Invention
In order to solve the problems of the dental repair material in the prior art, the invention provides a dental repair material containing ceramic wetting resin, and raw materials for preparing the dental repair material comprise acrylate monomer resin, ceramic wetting resin and inorganic powder filler;
the ceramic wetting resin is a mixture of inorganic materials and organic substances, and the inorganic materials include but are not limited to: quartz powder, barium glass powder, lanthanum glass powder, borosilicate glass powder, silicon oxide-zirconium oxide composite powder, silicon oxide-ytterbium oxide composite powder, nano silicon oxide powder, nano zirconium oxide powder and titanium oxide powder, wherein organic materials comprise but are not limited to polycarbonate, polyepoxide, polymerized methacrylic resin and polymer containing propionate groups, and the mass fraction of the inorganic materials in the ceramic wetting resin is 50-80%.
The ceramic wetting resin is added into the resin material, and the organic powder in the ceramic wetting resin can increase the wetting performance of the polymerized monomer on the powder, so that the monomer is guided to wet the filler powder, and meanwhile, the organic powder can coat the inorganic powder and has a certain modification effect on the surface of the inorganic powder. And the ceramic wetting resin is added, so that the processing operation performance is good (no sticking to instruments), the resin curing shrinkage rate is low, the mechanical property of the resin is good, and the color and the transparency meet the requirements.
The porcelain-wetting resin of the present invention usually contains other additives such as a color modifier in addition to inorganic materials and organic materials, and the inorganic materials, organic materials and other additives need to be uniformly mixed by stirring and kneading before use.
Preferably, the organic matter in the ceramic wetting resin is a mixture of bisphenol A glycerol dimethacrylate and triethylene glycol dimethacrylate, and the inorganic powder is barium glass powder and nano silicon dioxide.
More preferably, the porcelain moistening resin comprises 6-9 parts of bisphenol A glycerol dimethacrylate, 1-4 parts of triethylene glycol dimethacrylate, 28-32 parts of barium glass powder and 4-6 parts of nano silicon dioxide.
Preferably, the acrylic monomer resin comprises one or a combination of two of bisphenol a glycerol dimethacrylate (BisGMA), triethylene glycol dimethacrylate (TEGDMA), methacrylate (MMA), hydroxyethyl methacrylate (HEMA), urethane Dimethacrylate (UDMA), ethoxylated bisphenol a glycerol dimethacrylate (BisEMA), polyethylene glycol acrylate (PEGDMA), camphorquinone (EGDMA), alpha methyl cyanoacrylate, alpha butyl cyanoacrylate, or alpha decyl cyanoacrylate.
Further preferred is BisGMA, UDMA, TEGDMA or HEMA.
Preferably, the inorganic powder filler is one or more of quartz powder, barium glass powder, lanthanum glass powder, borosilicate glass powder, silicon oxide-zirconium oxide composite powder, silicon oxide-ytterbium oxide composite powder, nano silicon oxide powder, nano zirconium oxide powder and nano titanium oxide powder.
Further preferably one or more of barium glass powder, lanthanum glass powder and silicon oxide-zirconium oxide composite powder.
Preferably, the particle size of the inorganic powder is 0.5-50um.
Further preferably, the particle size of the inorganic powder is 0.5-2um.
Preferably, the mass of the acrylate monomer resin, the ceramic wetting resin and the inorganic powder filler is 5-40 parts of acrylic resin monomer, 5-40 parts of ceramic wetting resin powder and 30-80 parts of inorganic powder.
Preferably, the raw materials for preparing the dental restoration material further comprise an auxiliary agent, wherein the auxiliary agent is one or more of a fluorescent reagent, an indicator, an inhibitor, an accelerator, a viscosity regulator, a wetting agent, an antioxidant, a surfactant, a stabilizer and a diluent.
Preferably, the raw material for preparing the dental restorative material further comprises an initiator, and the initiator is camphorquinone, TPO or a mixture of the camphorquinone and the TPO.
The invention also provides a preparation method of the dental restoration material, which comprises the following steps:
1) Performing ball milling treatment on the porcelain moistening resin to obtain porcelain moistening resin powder;
2) Mixing the ceramic wetting resin subjected to ball milling treatment with other raw materials except the inorganic powder filler, and fully stirring by using double-planet stirring equipment;
3) And mixing the inorganic powder filler with the fully stirred materials, and treating the mixture by using a screw type kneader.
Preferably, the ball milling treatment can be dry ball milling or wet ball milling; and/or the presence of a gas in the atmosphere,
the ball milling auxiliary agent of the wet ball milling is a volatile organic compound, preferably one or a combination of methanol, ethanol and isopropanol; and/or the presence of a gas in the gas,
the mass ratio of the porcelain moistening resin to the grinding balls to the ball milling auxiliary agent is (1-2); and/or the presence of a gas in the gas,
after wet ball milling is finished, drying the ball-milled mixture by rotary evaporation at the temperature of 20-100 ℃, preferably 30-80 ℃; and/or the presence of a gas in the gas,
the ball milling adopts agate or zirconia grinding balls.
Preferably, the double planetary stirring speed is 5-20rpm; stirring at 10-60 deg.C, preferably 60 deg.C for 1-4hr; and/or the presence of a gas in the gas,
in the kneading process, the length-diameter ratio of a screw of the kneader is 5-50, and the rotating speed is 5-200rpm.
The invention has the following beneficial effects:
compared with the traditional material, the ceramic wetting resin is used, so that the silanization process can be omitted, the uniformity of the material is greatly improved, the shrinkage rate of the composite resin is effectively reduced, the optical and aesthetic effects of the composite resin are improved, and the mechanical strength of the composite resin is improved.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The porcelain-wetting resins mentioned in the examples were obtained from Liaoning AierChuang biomaterials Co.
Examples
The embodiment relates to a dental repair material which comprises the following raw materials in parts by weight:
TABLE 1
The specific components of the porcelain-moistening resin in the above examples are shown in table 2:
TABLE 2 (Unit g)
| Color of A1 | Color A2 | Color B1 | Tr color | |
| BisGMA | 7 | 7 | 8 | 8 |
| TEGDMA | 3 | 3 | 2 | 2 |
| Barium glass powder | 30 | 30 | 30 | 30 |
| Nano silicon dioxide | 5 | 5 | 5 | 5 |
| Iron oxide red | 0.02 | 0.04 | 0.02 | - |
| Iron oxide yellow | 0.01 | 0.02 | 0.04 | - |
| Titanium white powder | 0.01 | 0.01 | 0.01 | - |
The preparation method of the dental restoration material in the embodiment 1 comprises the following steps:
(1) Selecting A1 color-moistening porcelain resin;
(2) Dry-grinding the porcelain blocks with ball milling ball for 4hr;
(3) Stirring the monomer resin and the porcelain moistening resin by a double-planet stirrer at the stirring speed of 20rpm and the temperature of 60 ℃ for 4 hours;
(4) The above materials were mixed with fillers using a screw kneader with a screw length to diameter ratio of 50 and a rotation speed of 200rpm.
The preparation method of the dental restoration material described in the embodiments 2 to 4 is as follows:
(1) Selecting ceramic wetting resin
(2) Wet grinding the porcelain body and ball-milling balls for 4h, wherein the mass ratio of resin raw materials to the grinding balls to the ball-milling auxiliary agent is 1.
(3) Mixing and stirring monomer resin (shown in the table) and ceramic wetting resin with a double planetary stirrer at a stirring speed of 20rpm and a temperature of 60 ℃ for 4hr;
(4) The above materials were mixed with fillers using a screw kneader with a screw length-diameter ratio of 50 and a rotation speed of 200rpm.
Comparative example 1 the dental restorative material was prepared by the method of:
1) Mixing the monomer resin and the auxiliary agent, stirring with double planet at 20rpm and 60 deg.C for 4hr.
2) The above materials were mixed with fillers using a screw kneader with a screw length-diameter ratio of 50 and a rotation speed of 200rpm.
Comparative example 2 the dental restorative material was prepared by the method of:
1) Mixing the monomer resin and the auxiliary agent, stirring with a double-row planetary stirring speed of 20rpm at 60 deg.C for 4hr.
2) The above materials were mixed with fillers using a screw kneader with a screw length-diameter ratio of 50 and a rotation speed of 200rpm.
Comparative example 3 the dental restorative material was prepared by the method of:
1) Mixing the monomer resin and the auxiliary agent, and stirring with a double planetary stirrer at 20rpm and 60 deg.C for 4hr.
2) The above materials were mixed with fillers using a screw kneader with a screw length-diameter ratio of 50 and a rotation speed of 200rpm.
Comparative example 4
Compared with the examples 1 to 4, the dental material of the comparative example has a different preparation method without screw kneading, and comprises the following steps:
1) Mixing the monomer resin, the ceramic wetting resin and the auxiliary agent, and stirring for 4hr by adopting a double-planet stirrer pair at the stirring speed of 20rpm and the temperature of 60 ℃.
2) The above materials were mixed with fillers using a double planetary mixer at 50rpm.
Examples of the experiments
The experimental example relates to the performance detection of shrinkage, mechanical properties, light transmittance and color change of the tree material of the invention:
the shrinkage is the volume change after 14 days of reaction;
the detection method of the mechanical property comprises the following steps: the flexural strength was carried out in accordance with the method specified in YY 1042-2011 at 7.11, resulting in compliance with the requirement of 2.4. The compression performance is determined according to the compression performance of GB/T1041-2008 plastic, and the size of the sample is a cylinder with the diameter of 4mm and the height of 6-10 mm.
The maximum value of the color difference of the composite material in the dental material, which changes with time, based on L a b color system is more than or equal to 2 and less than or equal to 15; l is luminance data, a is red-blue hue data, and b is yellow-green hue data.
The results are shown in tables 3 and 4:
TABLE 3
According to the data, the mechanical property and the shrinkage rate of the material are improved to a certain degree after the ceramic wetting resin is added.
TABLE 4
As can be seen from the examples and comparative examples, the brightness of the transparent resin is improved, the red and yellow hues in the hues are lower, and the color interference is weak, while the colors of A1, A2 and B1 are normal and the brightness (L) is improved.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (10)
1. The dental restoration material containing ceramic wetting resin is characterized in that raw materials for preparing the dental restoration material comprise acrylate monomer resin, ceramic wetting resin and inorganic powder filler;
the ceramic wetting resin is a mixture comprising an inorganic material and an organic substance, the inorganic material is one or more of quartz powder, barium glass powder, lanthanum glass powder, borosilicate glass powder, silicon oxide-zirconium oxide composite powder, silicon oxide-ytterbium oxide composite powder, nano silicon oxide powder, nano zirconium oxide powder or titanium oxide powder, and the organic material is one or more of polycarbonate, polyepoxide, polymerized methacrylic resin or a polymer containing propionate groups; the mass fraction of the inorganic material in the ceramic wetting resin is 50-80%.
2. The dental restorative material of claim 1, wherein the acrylic monomer resin comprises one or a combination of two of bisphenol-a glycerol dimethacrylate, triethylene glycol dimethacrylate, methacrylate, hydroxyethyl methacrylate, urethane dimethacrylate, ethoxylated bisphenol-a glycerol dimethacrylate, polyethylene glycol acrylate, ethylene glycol dimethacrylate, camphorquinone, alpha methyl cyanoacrylate, alpha butyl cyanoacrylate, or alpha decyl cyanoacrylate; preferably one or more of bisphenol A glycerol dimethacrylate, urethane dimethacrylate, triethylene glycol dimethacrylate or hydroxyethyl methacrylate.
3. The dental restoration material according to claim 1 or 2, wherein the inorganic powder filler is one or more of quartz powder, barium glass powder, lanthanum glass powder, borosilicate glass powder, silica-zirconia composite powder, silica-ytterbium oxide composite powder, nano silica powder, nano zirconia powder and nano titania powder.
4. Dental restorative material according to any of claims 1-3, characterized in that the particle size of the inorganic powder is 0.5-50um, preferably 0.5-2um.
5. The dental restoration material according to any one of claims 1 to 4, wherein the acrylate monomer resin, the porcelain-wetting resin and the inorganic powder filler are, by mass, 5 to 40 parts of an acrylic resin monomer, 5 to 40 parts of porcelain-wetting resin powder and 30 to 80 parts of inorganic powder.
6. The dental restoration material according to any one of claims 1 to 5, wherein the raw materials for preparing the dental restoration material further comprise an auxiliary agent, wherein the auxiliary agent is one or more of a fluorescent agent, an indicator, an inhibitor, an accelerator, a viscosity regulator, a wetting agent, an antioxidant, a surfactant, a stabilizer and a diluent.
7. The dental restorative material of any of claims 1-5, wherein the raw materials for making the dental restorative material further comprise an initiator, wherein the initiator is camphorquinone, TPO, or a mixture of both.
8. A method for producing a dental restorative material as defined by any of claims 1 to 7, comprising the steps of:
1) Performing ball milling treatment on the porcelain moistening resin to obtain porcelain moistening resin powder;
2) Mixing the ceramic wetting resin subjected to ball milling treatment with other raw materials except the inorganic powder filler, and fully stirring by using double-planet stirring equipment;
3) And mixing the inorganic powder filler with the fully stirred materials, and treating the mixture by using a screw type kneader.
9. The preparation method according to claim 8, wherein the ball milling treatment is dry ball milling or wet ball milling; and/or the presence of a gas in the gas,
the ball milling auxiliary agent of the wet ball milling is a volatile organic compound, preferably one or a combination of methanol, ethanol and isopropanol; and/or the presence of a gas in the gas,
the mass ratio of the porcelain moistening resin to the grinding balls to the ball-milling auxiliary agent is 1-2, and the ball-milling time is 2-4 hr; and/or the presence of a gas in the gas,
after wet ball milling is finished, drying the ball-milled mixture by rotary evaporation at the temperature of 20-100 ℃, preferably 30-80 ℃; and/or the presence of a gas in the gas,
the ball milling adopts agate or zirconia grinding balls.
10. The production method according to claim 8 or 9, wherein the double planetary stirring speed is 5 to 20rpm; stirring at 10-60 deg.C, preferably 60 deg.C for 1-4hr; and/or in the kneading process, the length-diameter ratio of a screw of the kneader is 5-50, and the rotating speed is 5-200rpm.
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