CN113081859A - Anti-staining hard resin denture and preparation method thereof - Google Patents
Anti-staining hard resin denture and preparation method thereof Download PDFInfo
- Publication number
- CN113081859A CN113081859A CN202110276248.0A CN202110276248A CN113081859A CN 113081859 A CN113081859 A CN 113081859A CN 202110276248 A CN202110276248 A CN 202110276248A CN 113081859 A CN113081859 A CN 113081859A
- Authority
- CN
- China
- Prior art keywords
- denture
- grinding
- hard resin
- staining
- polishing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/20—Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
- A61K6/76—Fillers comprising silicon-containing compounds
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Dental Preparations (AREA)
Abstract
The application provides a preparation method of an anti-staining hard resin denture, which comprises the steps of material preparation, hot press molding, heat treatment and grinding and polishing, wherein the steps of grinding and polishing comprise: mechanically grinding the burr false tooth obtained after hot press molding and heat treatment by adopting a mixed abrasive material to obtain the hard resin false tooth with dyeing resistance; the flash denture comprises a resin base and at least 30 wt% of an inorganic filler; the mixed abrasive comprises a first material and a second material in a mass ratio of (45-60): (0.5-2), wherein the Vickers hardness of the first material is 20-50 HV, and the Rockwell hardness of the second material is 80-95 HRA. The preparation method provided by the application aims at the hard resin false tooth containing the inorganic filler, and the hard resin false tooth with higher hardness and remarkably improved staining resistance is prepared and obtained by adopting a specific mixed abrasive grinding mode in the grinding and polishing steps, so that the problem that the staining resistance of the high-hardness false tooth is difficult to improve at present is solved.
Description
Technical Field
The application relates to the technical field of denture materials, in particular to an anti-staining hard resin denture and a preparation method thereof.
Background
Currently, a widely used artificial tooth in clinical practice is a resin tooth, which is mainly composed of an enamel layer and a dentin layer. The traditional common synthetic resin tooth takes polymethyl methacrylate (PMMA) as a main material, has the advantages of low density, high toughness and difficult fracture compared with porcelain teeth, but has low strength, low hardness and poor wear resistance.
In order to improve the hardness and wear resistance of resin teeth, composite resin teeth, such as hard synthetic resin teeth, are generally made by adding inorganic fillers to resin materials. Hard synthetic resin teeth belong to medium and high-end products in the market, and inorganic fillers and resin matrixes are used in the enamel layer of the teeth, so that the hard synthetic resin teeth have the technical advantage that the hardness is obviously higher than that of common PMMA resin teeth. However, the existing hard synthetic resin teeth have a significant drawback in that they have poor staining resistance and are very significantly reduced during use. The enamel layer of the hard synthetic resin tooth is easy to stain, which directly leads to that the user who wants to pursue high hardness and high wear resistance has to sacrifice the requirement of staining resistance, thus reducing the use experience, and meanwhile, the enamel layer is a defect which is not negligible for the patient who has the requirement of beauty. Therefore, in the case of the conventional hard synthetic resin teeth, the staining problem becomes more prominent as the use time thereof is prolonged, the initially white teeth become yellow, red or gray, and the surface color of the stained denture shows more complicated changes depending on eating habits, and it has to be considered to perform the denture restoration again, which increases the time and cost for the patient's treatment, resulting in economic burden.
For hard synthetic resin teeth containing inorganic filler, the prior art has not yet provided a simple and effective composite resin denture capable of improving hardness and remarkably improving anti-staining capability and a preparation method thereof.
Disclosure of Invention
In order to solve the above problems, the present application aims to provide a hard resin denture capable of simultaneously having high hardness and high stain resistance.
In one aspect, the present application provides a method for preparing a hard resin denture with stain resistance, comprising the steps of preparing materials, hot press molding, heat treatment and grinding and polishing, wherein:
the grinding and polishing step comprises: mechanically grinding the burr false tooth obtained after hot press molding and heat treatment by adopting a mixed abrasive material to obtain the hard resin false tooth with dyeing resistance;
the flash denture comprises a resin base and at least 30 wt% of an inorganic filler;
the mixed abrasive comprises a first material and a second material in a mass ratio of (45-60): (0.5-2), wherein the Vickers hardness of the first material is 20-50 HV, and the Rockwell hardness of the second material is 80-95 HRA.
It is to be understood that "wt%" in this application is to be understood as a mass percentage.
In one embodiment, the step of grinding and polishing in the above-described manufacturing method may be applied to the treatment of a hard composite resin denture known in the art, such as a commercial synthetic resin tooth containing an inorganic filler.
The hard resin false tooth prepared by the preparation method provided by the application can show higher hardness under the condition of containing a certain content of inorganic filler. After the raw materials are subjected to hot press molding and heat treatment to prepare the rough-edged denture, the mixed abrasive is adopted for grinding and polishing, and particularly after the mixed abrasive with the hardness and the mass ratio is used for grinding and polishing, on one hand, the surface rough-edged defect of the formed denture can be fully removed, on the other hand, the obtained hard resin denture has lower surface roughness, higher surface smoothness and brightness and more compact surface fineness, so that the pore space of the surface of the material, which can be attached by dyeing substances, is reduced, and the color difference value of the denture before and after dyeing is remarkably reduced.
Wherein, for resin teeth containing inorganic filler, because the inorganic filler is mostly spherical small particles, and a plurality of gaps are arranged around the small particles, after the surface is mechanically polished and polished, the small particles are exposed, and then the surface becomes rough and uneven, and the resin teeth are more easily adhered and dyed by dyeing substances. In particular, silica powder or ultrafine silica powder having a small particle size is often used in the conventional art, and although it has good dispersibility in a resin and a large specific surface area, it has poor filling properties and a large number of voids exposed after being polished, which is disadvantageous in improving surface roughness and staining resistance.
According to the preparation method provided by the application, two kinds of grinding materials with very large hardness difference are adopted to be matched with the addition mass ratio for grinding and polishing, and experiments show that the effect of removing redundant wing edges or rough edges of the hard synthetic resin material in the process step during hot press molding can be ensured under the grinding and polishing mode of selecting two kinds of grinding materials with high hardness and low hardness for combination, the abrasion degree of the grinding materials on the surface of the hard synthetic resin material can be reduced, the surface roughness of the surface of the material caused by exposure of inorganic filler particles is reduced, and the dyeing resistance of the material is obviously improved.
Further, the first material comprises polymethyl methacrylate and the second material comprises alumina.
In one embodiment, the polymethyl methacrylate is added in the form of a polymethyl methacrylate synthetic resin containing not less than 95 wt% of polymethyl methacrylate, wherein the polymethyl methacrylate synthetic resin may be commercially available or self-made, and the Vickers hardness is 20HV to 50 HV.
In one embodiment, the polymethylmethacrylate synthetic resin may take various shapes such as a spherical shape, a block shape, or an irregular shape as the abrasive.
In one embodiment, the polymethylmethacrylate synthetic resin is used as one of the mixed abrasives in the form of a denture, wherein the polymethylmethacrylate synthetic resin denture is prepared as follows:
mixing 95-99 wt% of polymethyl methacrylate, 0.5-2 wt% of methyl methacrylate and 0.01-0.3 wt% of pigment into a dough, injecting the dough into a denture mould, performing hot pressing solidification, and naturally cooling to obtain the polymethyl methacrylate synthetic resin denture with irregular dentiform shape.
In a preferred embodiment, the mixed abrasive is polymethyl methacrylate synthetic resin denture and alumina in a mass ratio of 50: 1.
Further, the burr denture and the mixed abrasive are added in a mass ratio of 1: (1-4).
Preferably, the mass ratio of the raw edge false tooth to the mixed abrasive is 1: 1.2 to 3.5, more preferably 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1: 1.64, 1:1.7, 1: 1.8, 1: 1.9, 1:2, 1:2.04, 1: 2.1, 1:2.2, 1:2.3, 1:2.4, 1:2.5, 1: 2.6, 1:2.7, 1:3. 1: 3.2.
More preferably, in the grinding and polishing step, the mass ratio of the flash denture, the polymethylmethacrylate synthetic resin denture and the alumina is 25: 50: 1.
further, the mechanical grinding treatment comprises the following steps: and placing the rough-edged denture and the mixed abrasive into a centrifugal grinder, and performing fine grinding and polishing for 30-60 minutes.
Preferably, the time for the fine grinding and polishing is 35-50 min, and more preferably 40 min.
Optionally, the above-mentioned fine grinding and polishing step is performed using a horizontal centrifuge.
Alternatively, a cleaning liquid conventional in the art, such as water containing a small amount of a detergent, may be used in performing the finish polishing.
Compared with other polishing methods, such as chemical polishing, electrolytic polishing, ultrasonic polishing and the like, the method for placing the raw edge false tooth and the mixed abrasive in the horizontal centrifuge to carry out fine grinding polishing is more beneficial to production operation, has low cost, can realize quantitative production, and does not introduce new production process risks.
Optionally, the inorganic filler includes, but is not limited to, one or more of silica, hydroxyapatite, zirconia, ceramic powder, glass powder, tricalcium phosphate, sodium fluoride, strontium fluoride, lithium aluminum silicate, and borate, more preferably silica, and more preferably spherical silica powder particles;
optionally, the resin binder includes, but is not limited to, one or more of ethylene glycol dimethacrylate, urethane dimethacrylate, triethylene glycol dimethacrylate, dimethylaminoethyl methacrylate, and beta hydroxyethyl methacrylate.
Further, the inorganic filler comprises silicon dioxide, and the particle size of the silicon dioxide is 10-10000 nm.
Further, the burr denture comprises the following components in percentage by mass: 30 to 45 weight percent of silicon dioxide, 36 to 45 weight percent of ethylene glycol dimethacrylate and 17 to 25 weight percent of urethane dimethacrylate.
Preferably, the raw edge denture comprises the following components in percentage by mass: 35 to 42 weight percent of silicon dioxide, 38.9 to 43.3 weight percent of ethylene glycol dimethacrylate EDMA, 19.4 to 22 weight percent of urethane dimethacrylate UDMA and 0.01 to 0.3 weight percent of pigment.
Further, the silica is modified by a silane coupling agent, and the modification method comprises the following steps: and mixing the silicon dioxide with a modifying solution containing a silane coupling agent, and performing ball milling for 20-30 min.
Further, the modification method specifically comprises the following steps:
mixing silicon dioxide and ethanol, ball-milling for 20-30 h by using zirconia grinding beads, adding a mixed modification solution prepared from a silane coupling agent, glacial acetic acid and water, continuing ball-milling for 20-40 min by using the zirconia grinding beads, and performing rotary evaporation, drying, grinding and sieving to obtain the silica-based composite material.
In a preferred embodiment, the method for modifying silica specifically includes the steps of:
step a: mixing silicon dioxide with the particle size of 10-10000 nm with absolute ethyl alcohol, placing the mixture in a ball mill, and grinding the mixture for 20-30 hours at the rotating speed of 100-200 r/min by using zirconia grinding beads with the mass of 1.5-2 times of that of the silicon dioxide;
step b: silane coupling agent, glacial acetic acid and distilled water are mixed according to the following ratio of (3-8): (0.05-0.08): (1-3) mixing and uniformly stirring to obtain a modified liquid;
step c: adding the modifier obtained in the step b into the ball mill in the step a, and continuously grinding for 20-30 min, wherein the mass ratio of the silicon dioxide to the silane coupling agent is 100: (5-8);
step d: washing the ground silicon dioxide with absolute ethyl alcohol and performing rotary evaporation to obtain white spherical silicon dioxide powder, drying and rolling the powder and sieving the powder with a 120-mesh sieve for later use.
Optionally, the silane coupling agent is selected from one or more of vinyltrimethoxysilane, vinyltris (2-methoxyethoxy) silane, gamma-aminopropyltriethoxysilane, and gamma-glycidoxypropyltrimethoxysilane.
On one hand, the mode of performing ball-milling modification treatment on the silicon dioxide by using the silane coupling agent can graft silane molecules on the surface of the silicon dioxide, so that the similar compatibility and dispersibility of the silicon dioxide and a resin matrix are improved, the combination of the silicon dioxide and the resin matrix is facilitated, the composite material has a more compact tissue structure, and the hardness of the composite material is further improved.
On the other hand, in the method for silane modification of silicon dioxide in the prior art, the mixture of silicon dioxide and ethanol is mainly directly mixed with the coupling agent modification solution, and modification is carried out through ultrasonic dispersion or mechanical stirring, so that the aim of avoiding agglomeration of silicon dioxide powder is fulfilled. The ball milling modification method provided by the application not only can achieve the effect of uniform mixing through ultrasound or stirring, but also needs to add milling beads for ball milling, namely, zirconia milling beads are used for carrying out ball milling on silicon dioxide for a long time, then modification liquid is added, and the zirconia milling beads are used for continuing ball milling, even if the ball milling modification method has the mixing effect of grinding and rotating in the modification process, the silicon dioxide particles are enabled to be more uniform in size, the spherical surface is more uniform and the silane molecules are grafted tightly, further the dispersity is better when the silicon dioxide is blended with a resin matrix, a more compact and fastened combination surface is formed, and the advantage of improving the hardness of the silicon dioxide to the resin matrix is further played. Moreover, the particles exposed by the more uniformly dispersed silicon dioxide in the subsequent grinding and polishing process are tighter, which is beneficial to improving the grinding effect and further improving the staining resistance of the silicon dioxide when the silicon dioxide is ground by adopting the mixed abrasive in the subsequent process, otherwise, the silicon dioxide still has larger gaps, and the effect of improving the surface roughness of the false tooth by adopting the mixed abrasive in the subsequent process is weakened.
Further, in the method, the hot-press molding temperature is 110-120 ℃, the pressure is 6-8 MPa, the curing time is 5-20 min, and the cooling time is 5-10 min; the step of heat treating comprises: drying the mixture for 5 to 15 hours at the temperature of 80 to 100 ℃.
In a preferred embodiment, the preparation method specifically comprises the following steps:
the method comprises the following steps: preparing materials: carrying out silanization modification treatment on the silicon dioxide, and weighing ethylene glycol dimethacrylate, urethane dimethacrylate, the modified silicon dioxide and the pigment according to the mass percentage for later use;
step two: hot-press molding: injecting the prepared raw materials obtained in the step one into a hot-pressing die, filling the raw materials into a tooth dentin layer for hot-pressing forming, then cooling, filling the tooth enamel layer for hot-pressing forming, and then cooling and taking out to obtain the hard synthetic resin denture, wherein the hot-pressing forming temperature is 115 +/-5 ℃, the pressure is 6-8 MPa, the curing time is 10min, and the cooling time is 6 min;
step three: and (3) heat treatment: putting the hard synthetic resin false tooth obtained in the step two into a drying oven, drying for 10 hours at 90 +/-5 ℃, and taking out after natural cooling to obtain a rough-edged false tooth;
step four: grinding and polishing: and D, putting the mixed abrasive and the burr false tooth obtained in the step three into a horizontal centrifuge according to the mass ratio, and grinding and polishing for 30-60 min.
Wherein, the hot-press forming can make the raw material have the shape of the tooth, and the heat treatment can eliminate the internal stress of the false tooth after the hot-press forming. In one embodiment, the denture production process may further include steps of polishing, sorting, pasting, and packaging, which may all be performed by conventional operations and will not be described herein.
In another aspect, the present application also provides a hard resin denture resistant to staining prepared by the above preparation method.
On the other hand, the above method can be applied to the preparation of an enamel layer of a hard resin denture.
In another aspect, the present application also provides a mixed abrasive for treating a denture enamel layer containing an inorganic filler, the mixed abrasive comprising a first material and a second material in a volume ratio of (45-60): (0.5-2), the first material having a Vickers hardness of 20 HV-50 HV, and the second material having a Vickers hardness of 800 HV-1300 HV.
Preferably, the mixed abrasive comprises polymethyl methacrylate and alumina in a volume ratio of (45-60): (0.5-2).
Preferably, the polymethylmethacrylate is used in the form of a polymethylmethacrylate synthetic resin denture, which is prepared by the following method:
mixing 95-99 wt% of polymethyl methacrylate, 0.5-2 wt% of methyl methacrylate and 0.01-0.3 wt% of pigment into a dough, injecting the dough into a denture mould, performing hot pressing solidification, and naturally cooling to obtain the polymethyl methacrylate synthetic resin denture with irregular dentiform shape.
The following beneficial effects can be brought through the application:
the preparation method provided by the application aims at the hard resin false tooth containing the inorganic filler, and the hard composite resin material which simultaneously has higher hardness and remarkably improved staining resistance is prepared and obtained by adopting a specific mixed abrasive grinding mode in the grinding and polishing steps, so that the problem that the staining resistance of the high-hardness false tooth is difficult to improve at present is solved; according to experimental tests, the Vickers hardness of the hard resin denture obtained by the preparation method provided by the application is more than or equal to 35HV0.2, the color difference value delta E before and after the red yeast rice with the mass concentration of 0.2% is dyed for 24 hours is less than or equal to 6, the Vickers hardness of the existing hard resin denture product is about 30HV0.2, and the color difference value delta E before and after dyeing is more than or equal to 20; and the method is simple to operate and convenient for industrialization, does not introduce new impurities, and avoids pollution to the denture product.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a surface structure view under an optical microscope of a hard composite resin denture prepared in example 1 at a magnification of 500 times;
fig. 2 is a surface structure view under an optical microscope of the hard composite resin denture prepared in comparative example 1 at a magnification of 500 times;
FIG. 3 is a color change of a real object before and after red yeast is used for dyeing the hard composite resin denture prepared in example 1;
FIG. 4 is a color change of a real object before and after the hard composite resin denture prepared in comparative example 1 was dyed using red yeast rice.
Detailed Description
In order to more clearly explain the overall concept of the present application, the following detailed description of the overall scheme of the present invention is made by way of example. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
Unless otherwise specified, the starting components in the examples below are commercially available, and the laboratory instruments used are laboratory conventional laboratory instruments and the performance testing methods are those known in the art.
Examples 1 to 12
The series of embodiments provide a preparation method of an anti-dyeing hard composite resin material, which specifically comprises the following steps:
the method comprises the following steps: preparing materials: and according to the mass percentage, respectively weighing 41 percent of silicon dioxide, 39.5 percent of ethylene glycol dimethacrylate EDMA, 19.4 percent of carbamate dimethacrylate UDMA and 0.1 percent of pigment for later use, wherein the silicon dioxide is subjected to silanization modification treatment before weighing, and the specific treatment method is as follows:
step a: weighing 2kg of silicon dioxide powder with the particle size of 0.01-10000 nm by using an electronic balance, weighing 12-14L of absolute ethyl alcohol, pouring the absolute ethyl alcohol into the silicon dioxide powder for primary mixing in several times, wherein the primarily mixed silicon dioxide is not in a floating state and becomes transparent white small particles, stirring the mixture to fully mix the transparent white small particles for 30min, pouring the primarily mixed silicon dioxide into a 25L nylon tank, putting 3.5kg of zirconium oxide grinding beads into the nylon tank, placing the nylon tank on a ball mill for grinding for 24h, and setting the rotating speed to be 134 r/min;
step b: respectively weighing 125g of silane coupling agent KH570, 1.75g of glacial acetic acid and 50.75g of distilled water, mixing, and stirring with a magnetic stirrer for 25min to obtain a modifier after the liquids are fully and uniformly mixed;
step c: adding the modifier obtained in the step b into the ball mill in the step a, namely adding the modifier into the ethanol mixed solution of silicon dioxide, and continuing carrying out ball milling for 25min by using zirconia grinding beads;
step d: c, performing rotary evaporation on the mixed solution subjected to ball milling in the step c through a rotary evaporator to remove ethanol and water to obtain white spherical silicon dioxide powder, pouring the powder into a tray after the powder is cooled, cooling the powder for 10 to 24 hours, putting the powder into a drying oven at 105 ℃ for 12 hours, drying and cooling the powder, performing rolling compaction, and screening the powder by using a 120-mesh sieve for later use;
step two: hot-press molding: injecting the denture raw material prepared in the first step into a hot-pressing die, filling the denture raw material into a tooth dentin layer for hot-pressing forming, cooling, filling the denture raw material into a tooth enamel layer for hot-pressing forming, cooling and taking out to obtain the hard synthetic resin denture, wherein the hot-pressing forming temperature is 115 +/-5 ℃, the pressure is 6-8 MPa, the curing time is 10min, and the cooling time is 6 min;
step three: and (3) heat treatment: putting the hard synthetic resin false tooth obtained in the step two into a drying oven, drying for 10 hours at 90 +/-5 ℃, and taking out after natural cooling to obtain a rough-edged false tooth;
step four: grinding and polishing: and (3) enabling the raw edge false tooth and the grinding material obtained in the step three to be mixed according to the ratio of 1: (1-4) adding the mixture into a horizontal centrifugal grinder according to the mass ratio, and taking out after fine grinding and polishing for 40 min;
step five: and (4) sequentially carrying out polishing, classification inspection and plate pasting to obtain the hard resin false tooth with dyeing resistance.
The preparation methods of examples 1 to 12 were substantially the same, except that the material of the abrasive used in the fourth step and the mass ratio of the denture to the addition of the abrasive were different, and the selection of the type, hardness, morphology and volume ratio of the abrasive to be added were as shown in table 1.
Wherein, in the mixed abrasive of examples 1 to 7 in table 1, the polymethyl methacrylate PMMA is added in the form of polymethyl methacrylate synthetic resin denture, wherein the preparation method of the polymethyl methacrylate synthetic resin denture is as follows:
blending 98 wt% of polymethyl methacrylate, 1.8 wt% of methyl methacrylate and 0.2 wt% of pigment into a dough, injecting the dough into a denture mould for hot pressing and curing, and naturally cooling to obtain the polymethyl methacrylate synthetic resin denture with irregular tooth shape.
Example 13
This example is substantially the same as the preparation method of example 1, except that the silanization modification of silica in the raw material is carried out by ultrasonic dispersion, specifically: mixing silicon dioxide and absolute ethyl alcohol, performing ultrasonic dispersion for 1 hour, adding a modification solution, continuing ultrasonic dispersion for 3 hours, filtering, washing, drying and cooling in a drying box at 105 ℃ for 12 hours, rolling and sieving by using a 120-mesh sieve, wherein the steps, parameters and the like which are not mentioned are the same as those in example 1.
Comparative example 1
The present comparative example used the process for preparing hard synthetic resin teeth currently used by Shanghai pigeon oral Material Ltd, wherein the method of silanization modification of silica in the comparative example was the same as in example 12, and the alumina in example 12 was used as the abrasive in the fine grinding and polishing step.
And (3) performance testing:
the hard resin dentures obtained in the above examples were observed for surface appearance and tested for vickers hardness and staining resistance.
The hardness test method comprises the following steps:
1. sample preparation: carrying out parallel grinding on an occlusal surface and a tooth glaze surface of a tooth to be detected, wherein the thickness is more than 2 mm, the occlusal surface of the tooth is downward, and the tooth is placed in a mould for gypsum fixation;
2. polishing a test piece: grinding the bottom surface (the side with teeth of the plaster body) of the test piece smoothly by using No. P1000 abrasive paper, grinding the measuring surface by using No. P1500 abrasive paper, and measuring the level of the table surface of the teeth;
3. and (3) hardness testing: and (3) operating according to Vickers hardness tester operating instructions, selecting a hardness symbol HV0.2 to test, testing the hardness values of 3 points at different positions, recording the test results and calculating the average value of the test results.
Anti-staining test method:
1. weighing 0.1g of monascus pigment by using an electronic balance, dissolving the monascus pigment in water, preparing a monascus coloring agent with the mass concentration of 0.2%, uniformly stirring by using a glass rod, immersing the false tooth in the monascus coloring agent, sealing the opening of a beaker by using glass paper, and placing the beaker in a water bath at the temperature of (60 +/-1) ℃ for keeping the temperature for (23 +/-1) hours;
2. taking out the dyed false tooth, washing residual liquid of the dyeing agent attached to the surface of the false tooth by using distilled water until the false tooth is not decolored, and testing a color difference value delta E after drying for half an hour at room temperature, wherein the calculation formula is as follows:
△E*＝[(△L*)2+(△a*)2+(△b*)2]1/2
the results of the stain resistance test of the hard resin dentures obtained in each example are shown in table 1.
TABLE 1
As can be seen from the data in table 1, under the same conditions of the hard resin denture composition raw materials, the hot pressing process and the heat treatment method, different abrasives used in the grinding and polishing steps have a large influence on the staining resistance. Wherein, the mass ratio is 50: (0.8-1.2) grinding and polishing the mixed grinding material consisting of the polymethyl methacrylate synthetic resin false tooth and the aluminum oxide for 40min to obtain a bright and burr-free false tooth surface, wherein the color difference value delta E before and after dyeing for 24 hours by using 0.2% of red yeast rice is optimal and is only 5.83. And the inorganic filler silicon dioxide is subjected to silane modification by adopting a ball milling mode, so that the effect of improving the hardness of the denture is achieved, and meanwhile, the excellent synergistic auxiliary effect on the improvement of the staining resistance of the denture is achieved under the condition of combining with a specific abrasive. In the prior art, the vickers hardness of a conventional hard composite resin dental product is about 30HV0.2, and the color difference value delta E before and after red yeast rice dyeing with the mass concentration of 0.2% is greater than 20, namely, compared with the existing hard synthetic resin false tooth, the hard composite resin material provided by the application has remarkably improved dyeing resistance.
Wherein, the surface structure images of the hard composite resin false teeth of the example 1 and the comparative example 1 are respectively shown in fig. 1 and fig. 2, and it can be seen from the images that the tooth surface brightness and the surface fineness obtained in the example 1 are better and the tooth surface is not easy to be colored, while the tooth surface of the comparative example 1 has different density, the surface is not uniform and the damage is obvious, and the color difference is resisted.
Wherein, the real figures before and after the red yeast rice dyeing of the hard composite resin false tooth with the mass concentration of 0.2% for the example 1 and the comparative example 1 are respectively shown in fig. 3 and fig. 4, and as can be seen from the figures, the color depth of the false tooth of the example 1 after being dyed is obviously lower than that of the comparative example 1, which shows that the anti-dyeing property is obviously improved.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. A preparation method of an anti-staining hard resin denture comprises the steps of material preparation, hot press molding, heat treatment and grinding and polishing, and is characterized in that,
the grinding and polishing step comprises: mechanically grinding the burr false tooth obtained after hot press molding and heat treatment by adopting a mixed abrasive material to obtain the hard resin false tooth with dyeing resistance;
the flash denture comprises a resin base and at least 30 wt% of an inorganic filler;
the mixed abrasive comprises a first material and a second material in a mass ratio of (45-60): (0.5-2), wherein the Vickers hardness of the first material is 20-50 HV, and the Rockwell hardness of the second material is 80-95 HRA.
2. The method of manufacturing a stain resistant hard resin denture according to claim 1, wherein the first material comprises polymethylmethacrylate and the second material comprises alumina.
3. The method for producing a hard resin denture resistant to staining according to claim 1, wherein the flash denture and the mixed abrasive have a mass ratio of 1: (1-4).
4. The method for producing a hard resin denture resistant to staining according to claim 1, wherein the mechanical grinding treatment is: and placing the rough-edged denture and the mixed abrasive into a centrifugal grinder, and performing fine grinding and polishing for 30-60 minutes.
5. The method for manufacturing a hard resin denture resistant to staining as claimed in claim 1, wherein the inorganic filler comprises silica, and the silica has a particle size of 10 to 10000 nm.
6. The method of producing a stain-resistant hard resin denture according to claim 5, wherein the flash denture comprises: 30 to 45 weight percent of silicon dioxide, 36 to 45 weight percent of ethylene glycol dimethacrylate and 17 to 25 weight percent of urethane dimethacrylate.
7. The method for producing a stain-resistant hard resin denture according to claim 5 or 6, wherein the silica is a silica modified with a silane coupling agent, and the modification method comprises: and mixing the silicon dioxide with a modifying solution containing a silane coupling agent, and performing ball milling for 20-30 min.
8. The method of manufacturing a stain-resistant hard resinous denture according to claim 7, wherein the modification method specifically comprises the steps of:
mixing silicon dioxide and ethanol, ball-milling for 20-30 h by using zirconia grinding beads, adding a mixed modification solution prepared from a silane coupling agent, glacial acetic acid and water, continuing ball-milling for 20-40 min by using the zirconia grinding beads, and performing rotary evaporation, drying, grinding and sieving to obtain the silica-based composite material.
9. The method for manufacturing a hard resin denture resistant to staining according to claim 1, wherein the hot press molding temperature is 110 to 120 ℃, the pressure is 6 to 8MPa, the curing time is 5 to 20min, and the cooling time is 5 to 10 min; the step of heat treating comprises: drying the mixture for 5 to 15 hours at the temperature of 80 to 100 ℃.
10. A hard resin denture resistant to staining, produced by the production method according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110276248.0A CN113081859B (en) | 2021-03-15 | 2021-03-15 | Anti-staining hard resin denture and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110276248.0A CN113081859B (en) | 2021-03-15 | 2021-03-15 | Anti-staining hard resin denture and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113081859A true CN113081859A (en) | 2021-07-09 |
| CN113081859B CN113081859B (en) | 2022-06-03 |
Family
ID=76667948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110276248.0A Active CN113081859B (en) | 2021-03-15 | 2021-03-15 | Anti-staining hard resin denture and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113081859B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101507687A (en) * | 2009-04-07 | 2009-08-19 | 李榕卿 | Preparation method of dentistry composite resin material capable of improving abrasion resistance and obdurability |
| CN102552046A (en) * | 2012-01-13 | 2012-07-11 | 东华大学 | Composite dental restoration resin with silica microspheres as filler and preparation method thereof |
| CN102973416A (en) * | 2012-12-07 | 2013-03-20 | 东华大学 | Preparation method of dental restoring resin taking silicon dioxide and cluster of silicon dioxide as stuffing |
| CN106726625A (en) * | 2016-12-28 | 2017-05-31 | 广西深雅医疗科技股份有限公司 | A kind of PEEK artificial teeth tooth composite and preparation method thereof |
| CN108743405A (en) * | 2018-06-14 | 2018-11-06 | 中国科学院金属研究所 | A kind of artificial tooth zirconium oxide/resin bionic composite material and preparation method thereof |
| CN109620442A (en) * | 2018-12-20 | 2019-04-16 | 四川华柚医疗器械有限公司 | A kind of novel artificial tooth and preparation method thereof |
| CN109987969A (en) * | 2019-04-29 | 2019-07-09 | 成都贝施美生物科技有限公司 | A kind of rapid soaking zirconium oxide artificial tooth dyeing liquor |
| CN111803385A (en) * | 2020-07-31 | 2020-10-23 | 长沙博谱科学仪器有限公司 | Medical cosmetic denture material and preparation method thereof |
-
2021
- 2021-03-15 CN CN202110276248.0A patent/CN113081859B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101507687A (en) * | 2009-04-07 | 2009-08-19 | 李榕卿 | Preparation method of dentistry composite resin material capable of improving abrasion resistance and obdurability |
| CN102552046A (en) * | 2012-01-13 | 2012-07-11 | 东华大学 | Composite dental restoration resin with silica microspheres as filler and preparation method thereof |
| CN102973416A (en) * | 2012-12-07 | 2013-03-20 | 东华大学 | Preparation method of dental restoring resin taking silicon dioxide and cluster of silicon dioxide as stuffing |
| CN106726625A (en) * | 2016-12-28 | 2017-05-31 | 广西深雅医疗科技股份有限公司 | A kind of PEEK artificial teeth tooth composite and preparation method thereof |
| CN108743405A (en) * | 2018-06-14 | 2018-11-06 | 中国科学院金属研究所 | A kind of artificial tooth zirconium oxide/resin bionic composite material and preparation method thereof |
| CN109620442A (en) * | 2018-12-20 | 2019-04-16 | 四川华柚医疗器械有限公司 | A kind of novel artificial tooth and preparation method thereof |
| CN109987969A (en) * | 2019-04-29 | 2019-07-09 | 成都贝施美生物科技有限公司 | A kind of rapid soaking zirconium oxide artificial tooth dyeing liquor |
| CN111803385A (en) * | 2020-07-31 | 2020-10-23 | 长沙博谱科学仪器有限公司 | Medical cosmetic denture material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113081859B (en) | 2022-06-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kilinc et al. | Optical behaviors of esthetic CAD-CAM restorations after different surface finishing and polishing procedures and UV aging: An in vitro study | |
| WO2002015847A1 (en) | Dental curable composition | |
| JPS61134307A (en) | Dental restorative material | |
| Karadaş et al. | Evaluation of color stability and surface roughness of bulk-fill resin composites and nanocomposites | |
| Gad et al. | Translucency of nanoparticle-reinforced PMMA denture base material: An in-vitro comparative study | |
| Manjuran et al. | An in vitro study to identify a ceramic polishing protocol effecting smoothness superior to glazed surface | |
| JPH09255516A (en) | Dental composite material | |
| JP2021535222A (en) | Glazing composition, sintering process and parts kit for dental zirconia articles | |
| Günal-Abduljalil et al. | The effect of resin cement shade and restorative material type and thickness on the final color of resin-matrix ceramics | |
| JPH09169613A (en) | Dental composite restorative material | |
| CN113081859B (en) | Anti-staining hard resin denture and preparation method thereof | |
| Khosravani et al. | Final colour of Ultratranslucent multilayered zirconia veneers, effect of thickness, and resin cement shade | |
| EP4082516A1 (en) | Dental filling and repairing material kit | |
| JP2000139959A (en) | Dental ceramic material | |
| Tokunaga et al. | Castable polymer-infiltrated ceramic network composite for training model tooth with compatible machinability to human enamel | |
| Abdulsattar | Assessment The Mechanical and Color Changes Properties of Denture Base Material After Reinforcement with Nanoparticles Material | |
| Mohamed et al. | Effect of surface finishing protocols on color and translucency of zirconia reinforced lithium silicate glass-ceramic after thermo-mechanical aging and different staining solutions | |
| Mourouzis et al. | Impact of erosion and aging simulation on chairside materials | |
| Ibrahem et al. | Optical Properties of Zirconia Monolithic Crowns Constructed Using Speed Sintering Cycle | |
| JP2005263648A (en) | Filler, composite resin by using the same and dental prosthesis by using composite resin | |
| Hammoudeh et al. | Effect of different surface and heat treatments on the surface roughness, crystallography, and phase composition of high translucency zirconia for monolithic restorations | |
| CN114159315B (en) | Bioactive adhesive material for repairing tooth hard tissue defect and preparation method thereof | |
| Yousef et al. | The Effect of substrate and resin cement shades on the optical properties of two ceramic laminate veneer materials | |
| Y Saber et al. | Effect of Repeated Heat-Pressing on Color and Translucency of Lithium Disilicate Glass Ceramic Crowns | |
| Bukhari | Mechanical and optical properties of machinable and pressable glass ceramic |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |