WO2019062144A1 - 透光率和颜色渐变的牙科材料的制备方法及其制备的产品 - Google Patents
透光率和颜色渐变的牙科材料的制备方法及其制备的产品 Download PDFInfo
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- WO2019062144A1 WO2019062144A1 PCT/CN2018/087109 CN2018087109W WO2019062144A1 WO 2019062144 A1 WO2019062144 A1 WO 2019062144A1 CN 2018087109 W CN2018087109 W CN 2018087109W WO 2019062144 A1 WO2019062144 A1 WO 2019062144A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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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
- A61K6/15—Compositions characterised by their physical properties
- A61K6/16—Refractive index
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/0003—Making bridge-work, inlays, implants or the like
- A61C13/0022—Blanks or green, unfinished dental restoration parts
-
- 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
- A61K6/15—Compositions characterised by their physical properties
- A61K6/17—Particle size
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/60—Preparations for dentistry comprising organic or organo-metallic additives
- A61K6/65—Dyes
-
- 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
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
- A61K6/77—Glass
-
- 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
- A61K6/78—Pigments
-
- 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
- A61K6/79—Initiators
-
- 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
-
- 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
- A61K6/836—Glass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/90—Fillers or reinforcements, e.g. fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/52—Heating or cooling
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/08—Artificial teeth; Making same
- A61C13/082—Cosmetic aspects, e.g. inlays; Determination of the colour
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/0002—Condition, form or state of moulded material or of the material to be shaped monomers or prepolymers
Definitions
- the present application relates to the field of dental restoration technology, and in particular to a method for preparing a dental material having light transmittance and color gradation and a product thereof.
- CAD/CAM technology has also been used in the field of dental technology.
- the CAD/CAM technology next to the dental chair is to place the computer-aided design and computer-aided manufacturing equipment on the dental chair.
- the doctor uses the digital technology to obtain the patient's tooth model, and the computer analyzes the data and the teeth.
- the dental chair side diagnosis and treatment technology can complete the restoration preparation at one time, no need for temporary restoration, reduce the number of patient visits, can significantly improve the precision and accuracy of the restoration, improve the success rate of the repair treatment; effectively reduce the traditional porcelain teeth and
- the problem of discoloration of the gums and inconsistency of the edges of the movable dentures significantly improves the satisfaction of the patient's treatment effect.
- the development of CAD/CAM next to dental chairs has also led to the advancement of supporting materials.
- commonly used composite materials mainly include: composite resin materials, resin-infiltrated ceramic composite materials, and polyetheretherketone (PEEK) materials.
- PEEK polyetheretherketone
- Natural teeth are composed of enamel and dentin. The two tissues are completely different in source and characteristics and have their own unique optical properties. Dentin constitutes the body of the tooth, has light-blocking properties, and the enamel covers the dentin. It has translucency and light transparency, which causes the light transmittance and color of the natural tooth to be gradually changed from the neck to the cut end.
- a prosthesis made of a single aesthetically pleasing composite resin material has a disadvantage of low light transmittance and color similarity compared with natural teeth.
- the multi-layer composite resin material comprises at least three layers of composite resin materials of different colors, that is, composite resin materials of the same kind of light transmittance, the composite resin materials of the respective layers are superposed on each other, and the composite resin materials of the respective layers are from the bottom layer.
- the color of the top layer changes sequentially, which in turn mimics the color of natural teeth, but does not reflect the gradual change of natural tooth transmittance; in addition, the existing multi-layer composite resin material has the disadvantage of low strength.
- the purpose of the present application is to provide a method for preparing a dental material having a light transmittance and a color gradation and a product thereof to achieve the purpose of improving the aesthetic effect and strength of the composite resin material.
- the specific technical solutions are as follows:
- the present application provides a method for preparing a dental material having light transmittance and color gradation, the method comprising:
- each of the composite resin material precursor powders comprises: weighing raw materials, the raw materials including resin monomers, fillers, The initiator and the coloring agent are mixed to obtain a composite resin material precursor powder, wherein the weight ratio of the filler to the resin monomer is 10:90-90:10, preferably 70:30-85:15, and the initiator weight It is 0.1-3%, preferably 0.1-2% by weight of the resin monomer, and the colorant weight is 0.001-0.2%, preferably 0.002-0.1%, based on the total weight of the resin monomer and the filler; the resin monomer includes an olefin bond Unsaturated monomer and/or epoxy resin;
- the first composite resin material precursor powder of the at least three different light transmittances in the composite resin material precursor powder of the at least three different light transmittances, the first composite resin material precursor powder is dry-formed under a pressure of 3-20 MPa, preferably 4-10 MPa, Obtaining a first green body; wrapping the first green body in the second composite resin material precursor powder in the at least three kinds of composite resin material precursor powders with different light transmittance, at 3-20 MPa, preferably Dry pressing molding under a pressure of 4-10 MPa to obtain a second green body; repeating the wrapping and dry pressing forming operation until the at least three composite resin material precursor powders are dry pressed to obtain light transmittance and color a gradual dental material preform preform, wherein the light transmittance of each layer of the precursor powder in the dental material preform body of the light transmittance and the color gradation is sequentially increased from the inside to the outside;
- the curing treatment conditions are a temperature of 115 to 185 ° C, preferably 131 to 171 ° C, a pressure of more than 160 MPa, preferably 160 to 300 MPa, more preferably 200 to 250 MPa, and a holding time of 0.5 to 4 h, preferably 0.5 to 3 h.
- the light transmittance and the color gradient of the dental material further have a multi-layer color, between the two adjacent layers of the composite resin material, the chromaticity difference based on the Lab color system is greater than or equal to 1, and less than or equal to 11;
- the maximum difference of the chromaticity difference based on the Lab color system between the composite resin materials of the non-adjacent layers in the light transmittance and the color grading dental material is greater than or equal to 2 and less than or equal to 15;
- a sum of chromaticity differences between all adjacent layers of the composite resin material in the light transmittance and color grading dental material, and a composite resin having the highest chromaticity among the light transmittance and color grading dental materials The difference in chromaticity between the material and the layer of composite resin material having the lowest chroma is not more than 2;
- ⁇ E is the chromaticity difference
- ⁇ L is the difference between the L values between the two layers
- ⁇ a is the difference between the a values between the two layers
- ⁇ b is the difference between the b values between the two layers.
- the light transmittance and the color grading dental material further have a multilayer transmittance, and the difference between the transmittance between the adjacent two layers and the color gradient of the dental material is 0.5-10%.
- the difference in light transmittance between two adjacent composite resin materials is 1-15%; and the visible light (wavelength of 550 nm) transmittance of a composite resin material having the highest light transmittance is 50-75%.
- the light transmittance of the composite resin material having the lowest light transmittance is 30-60%, and the other composite resin material having the highest light transmittance and the other composite resin material having the lowest light transmittance are
- the layer composite resin material has a light transmittance of 40 to 70%.
- the weight ratio of the filler to the resin monomer is 31:69-69:31, preferably 43:57-62:38, and the initiator weight is 0.1-3%, preferably 0.1% by weight of the resin monomer. -2%, the colorant weight is 0.001-0.2%, preferably 0.002-0.1% of the total weight of the resin monomer and the filler;
- the heat curing treatment conditions are a temperature of 115 to 169 ° C, preferably 155 to 165 ° C, a pressure of 210 to 300 MPa, preferably 240 to 290 MPa, and a holding time of 1.1 to 1.8 h, preferably 1.6 to 1.8 h.
- the raw material is mixed to obtain a composite resin material precursor powder, including:
- the raw material is mixed with a ball milling aid, and the composite resin material precursor powder is prepared by a ball milling method, wherein the mass ratio of the raw material: grinding ball: ball milling aid is (1:1:1)-(3:6:2), preferably For 2:4:1, the ball milling time is 0.5-2h.
- the filler has a particle size ranging from not more than 2.5 ⁇ m, preferably not more than 2 ⁇ m, more preferably from 0.05 to 2 ⁇ m; and the filler has a refractive index of from 1.40 to 1.7, preferably from 1.45 to 1.6.
- the raw material further comprises a polymerization inhibitor, and the polymerization inhibitor accounts for 0.1-3%, preferably 0.2-2%, of the total weight of the resin monomer.
- the raw material further comprises an accelerator, the accelerator comprising 0.1-3%, preferably 0.2-2%, based on the total weight of the resin monomer.
- the raw material further comprises at least one of a fluorescent-imparting agent, an indicator, an inhibitor, an accelerator, a viscosity modifier, a wetting agent, an antioxidant, a surfactant, a stabilizer, and a diluent.
- a fluorescent-imparting agent an indicator, an inhibitor, an accelerator, a viscosity modifier, a wetting agent, an antioxidant, a surfactant, a stabilizer, and a diluent.
- the filler may further comprise nanoparticles, wherein the nanoparticles comprise 1-25%, preferably 1-15% by weight of the filler; the nanoparticles have an average diameter of 35-100 nm, preferably It is 40-50nm.
- the raw material further comprises reinforcing fibers, the reinforcing fibers are 1-30%, preferably 1-10% by weight of the filler; and the reinforcing fibers have a diameter of 0.1-25 ⁇ m, preferably 0.5-10 ⁇ m.
- the reinforcing fiber has a length of 0.001 to 1 mm, preferably 0.1 to 0.5 mm; the reinforcing fiber has a refractive index of 1.4 to 1.7, preferably 1.45 to 1.6; and the reinforcing fiber comprises glass fiber, quartz fiber, and silicon.
- the raw material is mixed to obtain a composite resin material precursor powder, including:
- the resin monomer, the filler, the initiator and the coloring agent other than the reinforcing fiber are mixed and then ball-milled to obtain a raw material mixture, wherein the raw material: grinding ball: ball milling aid has a mass ratio of 1:1:1-3: 6:2, preferably 2:4:1, ball milling time is 0.5-2h;
- the raw material mixture is mixed with the reinforcing fibers to obtain a composite resin material precursor powder.
- the coloring agent comprises one or a combination of a red coloring agent, a yellow coloring agent and a black coloring agent, wherein the red coloring agent accounts for 0.001-0.06%, preferably iron oxide, of the weight of the raw material.
- Red preferably iron oxide
- yellow coloring agent comprises 0.001-0.04% by weight of the raw material, and comprises one or a combination of iron oxide yellow, yttrium yellow, vanadium zirconium yellow, and yttrium yellow
- the black coloring agent occupies the raw material 0-0.03% by weight, preferably iron oxide black.
- the present application also provides a light-transmitting and color-grading dental material prepared by the above method.
- the light transmittance and color grading dental material prepared by the method provided by the present application have extremely high flexural strength, and the flexural strength reaches 248 MPa or more as determined experimentally.
- the light transmittance and color grading dental material prepared by the method provided by the present application have extremely high compressive strength, and the compressive strength has reached 581 MPa or more as determined by experiments.
- the light transmittance and color gradient dental material prepared by the method provided by the present application can effectively improve the aesthetic effect of the restoration, so that the color and transparency are gradually changed in the height direction, and the cut end and the neck of the natural tooth are better simulated. Aesthetic characteristics.
- the embodiment of the present application provides a method for preparing a dental material with light transmittance and color gradation, including:
- each of the composite resin material precursor powders comprises: weighing raw materials, the raw materials including resin monomers, fillers, The initiator and the coloring agent are mixed to obtain a composite resin material precursor powder, wherein the weight ratio of the resin monomer to the filler is 10:90-90:10, preferably 70:30-85:15, and the initiator weight It is 0.1-3%, preferably 0.1-2% by weight of the resin monomer, and the colorant weight is 0.001-0.2%, preferably 0.002-0.1%, based on the total weight of the resin monomer and the filler; the resin monomer includes an olefin bond Unsaturated monomers and / or epoxy resins.
- the resin monomer may be selected from polymerizable ethylenically unsaturated monomers with or without acid functional groups, such as acrylates, methacrylates, hydroxy-functional acrylates, hydroxy-functionalized nails. One or a combination of acrylates.
- the resin monomer may also use a polymerizable resinizable monomer other than methacrylate, such as an epoxy resin such as polyethylene glycol dimethacrylate (PEGDMA), bisphenol A-dimethacrylic acid. Glycidyl ester (Bis-GMA), urethane dimethacrylate (UDMA), triethylene glycol dimethacrylate (TEGDMA), ethoxylated bisphenol A dimethacrylate (Bis-EMA6) And one or a combination of hydroxyethyl methacrylate (HEMA), bisphenol A epoxy resin (epoxy resin E-44).
- an epoxy resin such as polyethylene glycol dimethacrylate (PEGDMA), bisphenol A-dimethacrylic acid. Glycidyl ester (Bis-GMA), urethane dimethacrylate (UDMA), triethylene glycol dimethacrylate (TEGDMA), ethoxylated bisphenol A dimethacrylate (Bis-EMA6) And one or a combination of
- the resin monomer may also be a mixture of an ethylenically unsaturated monomer and an epoxy resin.
- the epoxy resin can be from 5 to 30% by weight of the ethylenically unsaturated monomer.
- a resin monomer can be obtained according to the following formulation.
- Bis-GMA 0-70%, preferably 0-30%;
- UDMA 10-70%, preferably 40-60%;
- Bis-EMA6 0-50%, preferably 0-30%;
- Epoxy resin E-44 0-40%, preferably 0-20%;
- TEGDMA 10-60%, preferably 20-40%;
- HEMA 0-50%, preferably 0-20%.
- the filler has a particle size ranging from not more than 2.5 ⁇ m, preferably not more than 2 ⁇ m, more preferably from 0.05 to 2 ⁇ m; and the filler has a refractive index of from 1.40 to 1.7, preferably 1.45. -1.6.
- the filler may also have a certain size fraction, for example, a portion of the filler may have a particle size ranging from 0.1 to 1 ⁇ m, and another portion of the filler may have a particle size ranging from less than 0.1 ⁇ m. Having a certain particle size grading of the filler allows the light transmittance and color grading of the dental material to have better polishing and abrasion resistance.
- the filler may be an inorganic material, including but not limited to: quartz powder, bismuth glass powder, bismuth glass powder, borosilicate glass powder, silica-zirconia composite powder, silica-yttria composite powder. , nano-silica powder, nano-zirconia powder, nano-titanium oxide powder.
- the filler may also be an organic filler including, but not limited to, a polycarbonate powder filled with an inorganic material, a polyepoxide powder, a polymerized methacrylic resin powder, and a polycarbonate powder not filled with an inorganic material, Polyepoxide powder, polymerized methacrylic resin powder.
- the initiator includes, but is not limited to, one of dicumyl peroxide, t-butyl peroxide, benzoyl peroxide, tert-butyl peroxyacetate, t-butyl peroxybenzoate or a combination thereof.
- the filler in order to increase the bonding strength between the filler and the polymerized monomer, is subjected to surface modification treatment with a coupling agent before being mixed with other raw materials.
- Coupling agents which may be used include, but are not limited to, ⁇ -methacryloxypropyltrimethoxysilane KH-570, ⁇ -mercaptopropyltriethoxysilane KH-580, ⁇ -aminopropyltrimethoxysilane JH-A111 and so on.
- the treatment of the surface of the filler with a coupling agent enhances the bonding strength between the filler particles and the polymerized monomer, such as an ethylenically unsaturated monomer, thereby increasing the hardness of the restoration.
- the raw material is mixed to obtain a composite resin material precursor powder, comprising: mixing the raw material with a ball milling aid, and preparing a composite resin material precursor powder by a ball milling method, wherein the raw material: Grinding ball: The mass ratio of the ball milling aid is (1:1:1)-(3:6:2), preferably 2:4:1, and the ball milling time is 0.5-2 h.
- the process conditions of the ball mill mixture may be: using agate or zirconia grinding balls, and the ball milling aid is a volatile organic substance such as one of methanol, ethanol, acetone or a combination thereof.
- the mixture obtained by ball milling and mixing can be subjected to a rotary evaporation and drying process to prepare a composite resin material precursor powder having a light transmittance and a color gradation, wherein the temperature during rotary evaporation is 20-100 ° C, preferably 30-80. °C is further preferably 45-58 °C.
- the temperature at the time of drying is 20 to 100 ° C, preferably 30 to 80 ° C, and more preferably 45 to 58 ° C.
- the preparation of the composite resin material precursor powder according to the above ball milling method can make the components in the composite resin material precursor powder more uniformly mixed, can also improve the preparation efficiency, and can also facilitate the molding of the material.
- the ratio between the resin monomer, the filler, the initiator and the colorant in each composite resin material can be adjusted according to actual needs, thereby obtaining a composite resin material having different light transmittance.
- composite resin material precursor powder A having a light transmittance of 50-75%; composite resin material precursor powder B having a light transmittance of 40-70%; composite resin having a light transmittance of 30-60%
- the material precursor powder C wherein the light transmittance is measured by a light transmittance tester when the test light wavelength is 550 nm.
- the first method for obtaining a composite resin precursor powder having a specific light transmittance is: preparing a composite resin precursor powder of a plurality of formulations, and then curing the prepared precursor powder under a predetermined condition. Then, when the test light wavelength is 550 nm, the transmittance of the plurality of composite resin material precursor powders after curing is tested by a light transmittance tester, and then the prosthesis precursor corresponding to the light transmittance is selected according to the required light transmittance.
- the powder is formulated according to the formula to prepare a composite resin material precursor powder.
- the second is to use the empirical formula to calculate the light transmittance of each composite resin material precursor powder according to the nature and proportion of each component in the composite resin material precursor powder, and then select and transmit according to the required light transmittance.
- the formula of the prosthetic precursor powder corresponding to the rate is prepared, and the composite resin material precursor powder is prepared according to the formula.
- the composite resin material precursor powder C may be added to the mold in the order of light transmittance from low to high, and the upper surface of the precursor powder is flattened to be flat; and the composite resin material is further used.
- the precursor powder B is added to the mold, and the upper surface of the precursor powder is flattened to a flat state; the above composite resin material precursor powder A is added to the mold, and the upper surface of the precursor powder is flattened to be flat; 3-20 MPa, preferably 4-10 MPa under pressure, dry-pressed to obtain a dental material preform having a light transmittance and a color gradient;
- the composite resin material precursor powder C is dry-formed under a pressure of 3-20 MPa, preferably 4-10 MPa, to obtain a first green body; the first green body is wrapped in the composite resin material precursor powder B in the three different transmittance composite resin material precursor powders, at 3-20 MPa, preferably 4-10 MPa Pressing and forming under pressure to obtain a second green body; repeating the wrapping and dry pressing forming operation until the three composite resin material precursor powders are dry-formed to obtain a dental material with a light transmittance and a color gradient
- the curing treatment conditions are a temperature of 115 to 185 ° C, preferably 131 to 171 ° C, a pressure of more than 160 MPa, preferably 160 to 300 MPa, more preferably 200 to 250 MPa, and a holding time of 0.5 to 4 h, preferably 0.5 to 3 h.
- the thermal curing initiator is dicumyl peroxide, t-butyl peroxide, benzoyl peroxide, tert-butyl peroxyacetate, tert-butyl peroxybenzoate One or a combination thereof.
- the chromaticity difference between the adjacent two layers of the composite resin material precursor powder in the light transmittance and the color grading dental material preform body is based on the Lab color system. Greater than or equal to 1, and less than or equal to 11;
- the maximum value of the chromaticity difference based on the Lab color system is greater than or equal to 2, and less than or equal to 15;
- a sum of chromaticity differences between all adjacent layers of the composite resin material in the light transmittance and color grading dental material, and a composite resin having the highest chromaticity among the light transmittance and color grading dental materials The difference in chromaticity between the material and the layer of composite resin material having the lowest chroma is not more than 2;
- ⁇ E is the chromaticity difference
- ⁇ L is the difference between the L values between the two layers
- ⁇ a is the difference between the a values between the two layers
- ⁇ b is the difference between the b values between the two layers.
- the light transmittance and color grading dental material further has a multilayer transmittance, a transmittance between adjacent two layers of light transmittance and a color gradation of the dental material.
- the difference is 0.5-10%; the difference in light transmittance between two adjacent composite resin materials is 1-15%; and the transmittance of a composite resin material having the highest light transmittance is 50-75%
- the light transmittance of the layer of the composite resin material having the lowest light transmittance is 30-60%, and the other layer of the composite resin material having the highest light transmittance and the layer of the composite resin material having the lowest light transmittance are the other
- the light transmittance of each layer of the composite resin material is 40-70%.
- a composite resin material with moderate translucency belongs to the transition layer, which can be one layer or multiple layers;
- the light transmittance of the composite resin material precursor powder prepared by the following three kinds of composite resin material precursor powders and the color gradient of the dental material can be satisfied, and the chromaticity difference between the three composite resin material precursor powders needs to be satisfied.
- the conditions are explained.
- chromaticity difference is sometimes also referred to simply as “chromatic aberration.”
- the chromaticity of the three composite resin precursor powders is based on the Lab color system and is measured by a color difference meter or a spectrophotometer.
- the chromaticity of the first composite resin material precursor powder may be marked by L1, a1, b1; the chromaticity of the second composite resin material precursor powder may be marked by L2, a2, b2; labeled with L3, a3, b3
- the color of the three composite resin material precursor powders may be marked by L1, a1, b1; the chromaticity of the second composite resin material precursor powder may be marked by L2, a2, b2; labeled with L3, a3, b3 The color of the three composite resin material precursor powders.
- the inter-layer chromaticity difference ⁇ E is calculated, where ⁇ E is the chromaticity difference; ⁇ L is the difference between the L values between the two layers; ⁇ a is the difference between the a values between the two layers; and ⁇ b is the difference between the b values between the two layers.
- the first composite resin material precursor powder is used as the uppermost layer material
- the second composite resin material precursor powder is used as the intermediate transition layer
- the third composite resin material precursor powder is used as the lowermost layer material
- L1 ⁇ L2 ⁇ L3, a1 ⁇ a2 ⁇ a3, b1 ⁇ b2 ⁇ b3; the L value of the first composite resin material precursor powder, the second composite resin material precursor powder, and the third composite resin material precursor powder are decreased
- the trend when the a value and the b value have an increasing trend, can simulate the gradual change of the transmittance of the natural tooth.
- the chromaticity difference between the uppermost layer and the lowermost layer should be 2 or more and 15 or less; the chromaticity difference between the uppermost layer and the intermediate transition layer is 1 or more and 11 or less; the intermediate transition layer and The chromaticity difference between the lowermost layer is 1 or more and 11 or less, and the chromaticity difference between the uppermost layer and the lowermost layer - (the chromaticity difference between the intermediate transition layer and the lowermost layer + the most The chromaticity difference between the upper layer and the intermediate transition layer)
- the first composite resin material precursor powder L1 ranges from 62 to 80, a1 ranges from -2.2 to 2.2, and b1 ranges from 5 to 16, and the light transmittance ranges from 50 to 75%.
- the second composite resin material precursor powder L2 ranges from 58 to 76, a2 ranges from -2.0 to 2.5, and b2 ranges from 8 to 20, and the light transmittance ranges from 40 to 70%.
- the third composite resin material precursor powder L3 ranges from 53 to 72, a3 ranges from -1.8 to 2.8, and b3 ranges from 10 to 24, and the light transmittance ranges from 30 to 60%.
- the light transmittance and color grading of the dental material prepared by using the above three composite resin material precursor powders the light transmittance of the first composite resin material precursor powder as the uppermost layer is higher than that of the intermediate transition layer.
- the transmittance of the second composite resin material precursor powder; and the transmittance of the second composite resin material precursor powder as the intermediate transition layer is higher than that of the third composite resin material precursor powder as the lowermost layer Light transmittance of the body.
- the difference in chromaticity between adjacent layers is 2 or more and 15 or less, and between adjacent layers The chromaticity difference is 1 or more and 11 or less.
- the transmittance of each layer of the composite resin material from the lowermost layer to the uppermost layer is sequentially increased. High; or when the light transmittance of the uppermost layer of the restoration is the lowest, the light transmittance of each layer of the composite resin material from the lowermost layer to the uppermost layer is sequentially lowered.
- the upper and lower light transmittance and the color grading dental material prepared by using the composite resin material precursor powder having the above-mentioned inter-layer chromaticity difference can simulate the characteristics of natural tooth transmittance from the cut end to the neck light transmittance and color gradation. Further, the dental restoration is more beautiful.
- the above three composite resin material precursor powders can be used to prepare another dental material having a light transmittance and a color inside and outside gradation, and conditions for satisfying the chromaticity difference between the three composite resin material precursor powders are required. Be explained.
- the first composite resin material precursor powder having a chromaticity value of L1, a1, b1 is used as the outermost layer material; the second composite resin material precursor powder having a chromaticity of L2, a2, b2 is used as the secondary outer layer material;
- the third composite resin material precursor powder having a chromaticity of L3, a3, and b3 is used as the innermost layer material.
- the chromaticity difference between the outermost layer and the innermost layer should be 2 or more and 15 or less; the chromaticity difference between the outermost layer and the secondary outer layer is 1 or more and 11 or less; The chromaticity difference from the innermost layer is 1 or more and 11 or less, and the chromaticity difference between the outermost layer and the innermost layer - (the chromaticity difference between the outermost layer and the outer outer layer + the outer The chromaticity difference between the layer and the innermost layer)
- the light transmittance of the first composite resin material precursor powder as the outermost layer is higher than that of the second composite resin material precursor powder as the secondary outer layer;
- the light transmittance of the second composite resin material precursor powder is higher than that of the third composite resin material precursor powder which is the innermost layer.
- the dental material prepared by using the composite resin material precursor powder having the above-mentioned inter-layer chromaticity difference powder can simulate the gradual change of the light transmittance of the natural tooth from the inside to the outside, thereby making the dental prosthesis More beautiful.
- the raw material further includes a polymerization inhibitor, and the polymerization inhibitor accounts for 0.1-3%, preferably 0.2-2%, of the total weight of the resin monomer.
- the polymerization inhibitor includes, but is not limited to, one of 2,6-di-tert-butyl-p-cresol (BHT) and t-butyl hydroquinone (TBHQ) or combination.
- BHT 2,6-di-tert-butyl-p-cresol
- TBHQ t-butyl hydroquinone
- the raw material further includes an accelerator, the accelerator comprising 0.1-3%, preferably 0.2-2%, based on the total weight of the resin monomer.
- the promoter includes, but is not limited to, N,N-dimethyl-p-toluidine (DMT), N,N-dihydroxyethyl-p-toluidine (DHET), 4-dimethyl One or more combinations of ethylaminobenzoate (EDMAB) and N,N-dimethylaminoethyl methacrylate (DMAEMA).
- DMT N,N-dimethyl-p-toluidine
- DHET N,N-dihydroxyethyl-p-toluidine
- EDMAB ethylaminobenzoate
- DMAEMA N,N-dimethylaminoethyl methacrylate
- the raw material further includes a reagent for imparting fluorescence, an indicator, an inhibitor, an accelerator, a viscosity modifier, a wetting agent, an antioxidant, a surfactant, a stabilizer, and a diluent. At least one of them.
- the reagent for imparting fluorescence may be an azo fluorescent pigment, a tryptophan or a pyridine fluorescent pigment, etc.; the indicator may be a redox indicator or a wear indicator; the inhibitor may be a curing inhibitor or the like; the accelerator may be It is a photopolymerization accelerator or a thermal polymerization accelerator; the viscosity modifier may be paraffin wax or polyethylene wax; the wetting agent may be a silane agent; the antioxidant may be sodium ascorbate; and the surfactant may be octylphenol.
- the filler further includes nanoparticles, wherein the nanoparticles account for 1-25%, preferably 1-15% by weight of the filler; an average diameter of the nanoparticles It is 35-100 nm, preferably 40-50 nm.
- the dental material having a light transmittance and a color gradation can have an opalescent effect close to that of a natural tooth.
- the raw material further includes reinforcing fibers, the reinforcing fibers being 1-30%, preferably 1-10% by weight of the filler; and the reinforcing fibers having a diameter of 0.1- 25 ⁇ m, preferably 0.5-10 ⁇ m; the reinforcing fiber has a length of 0.001 to 1 mm, preferably 0.1 to 0.5 mm; the reinforcing fiber has a refractive index of 1.4 to 1.7, preferably 1.45 to 1.6; the reinforcing fiber comprises glass One or a combination of fibers, quartz fibers, siliceous fibers, ceramic fibers, and polymer fibers, which are preferably polyethylene fibers.
- the addition of reinforcing fibers to the raw material can improve the fracture toughness of the light-transmitting and color-grading dental materials.
- the reinforcing fiber is subjected to a cleaning treatment and a surface modification treatment before being mixed with other raw materials
- the cleaning method comprises: heat treatment cleaning, solvent soak cleaning or acid-base corrosion cleaning
- the modification treatment method includes : Modification of coupling agent, modification by plasma treatment and modification by chemical grafting treatment.
- the surface of the reinforcing fibers can be treated with a coupling agent.
- Coupling agents which may be used include, but are not limited to, ⁇ -methacryloxypropyltrimethoxysilane KH-570, ⁇ -mercaptopropyltriethoxysilane KH-580, ⁇ -aminopropyltrimethoxysilane JH-A111 and so on.
- the use of a coupling agent to treat the surface of the filler enhances the bonding strength between the fiber and the ethylenically unsaturated monomer, thereby increasing the hardness of the light-transmitting and color-grading dental material.
- the surface modification treatment of the reinforcing fibers can further improve the fracture toughness of the densities and the color gradient of the dental materials.
- the raw materials other than the reinforcing fibers may be ball-milled to obtain a raw material mixture; and the raw material mixture may be mixed with the reinforcing fibers to obtain a composite resin material precursor powder.
- the raw material is mixed to obtain a composite resin material precursor powder, including:
- the resin monomer, the filler, the initiator and the coloring agent other than the reinforcing fiber are mixed and then ball-milled to obtain a raw material mixture, wherein the raw material: grinding ball: ball milling aid has a mass ratio of 1:1:1-3: 6:2, preferably 2:4:1, ball milling time is 0.5-2h;
- the raw material mixture is mixed with the reinforcing fibers to obtain a composite resin material precursor powder.
- the coloring agent comprises one or a combination of a red coloring agent, a yellow coloring agent, and a black coloring agent, wherein the red coloring agent accounts for 0.001% of the weight of the raw material. 0.06%, preferably iron oxide red; the yellow colorant comprises 0.001-0.04% by weight of the raw material, and comprises one or a combination of iron oxide yellow, bismuth yellow, vanadium zirconium yellow and yellow enamel;
- the black colorant comprises from 0 to 0.03% by weight of the starting material, preferably iron oxide black.
- the colorant is generally a metal oxide such as iron oxide, zirconium oxide, vanadium oxide, and antimony oxide.
- the ratio of the red colorant, the yellow colorant, and the black colorant can be adjusted according to different practical needs, thereby preparing dental materials of different colors of light transmittance and color gradation.
- the embodiments of the present application also provide a light-transmitting and color-grading dental material prepared by using any of the above methods.
- Table 1 shows the formulation and process parameters of four kinds of composite resin material precursor powders with different light transmittance.
- the values corresponding to the resin monomer, filler, initiator and colorant in Table 1 are parts by weight, and each part by weight may be 100 g.
- Table 2 shows the chromaticity values and light transmittance of the powders 1-4 based on the Lab color system.
- the chromaticity values and the light transmittance corresponding to the powders 1-4 are shown in Table 2.
- the light transmittance of the powders 1-4 is sequentially decreased, wherein the chromaticity of the powders 1-4 is Based on the Lab color system, the above powder is solidified under a preset condition and measured by a color difference meter or a spectrophotometer.
- the light transmittance is measured by a light transmittance tester after the powder is cured under a predetermined condition and the test light wavelength is 550 nm.
- the powder 1 is added to the mold as the first layer, after the flattening, the powder 2 is added, and the powder 2 is used as the second layer, and after flattening, the powder 4 is added, and the powder 4 is taken as the third layer.
- the processing temperature is 115 ° C
- the pressure is 160 MPa
- the holding time is 0.5 h
- the three-layer light transmittance and color gradient can be prepared.
- the chromaticity difference between the first layer and the third layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The chromaticity difference between 1 is 1 or more and 11 or less, and the chromaticity difference between the first layer and the third layer - (the chromaticity difference between the first layer and the second layer + the second layer and the third layer The difference in chromaticity)
- the light transmittance and the color gradient of the dental material prepared by using the above three powders have a light transmittance of the first layer greater than that of the second layer; the light transmittance of the second layer is greater than the transmittance of the third layer
- the color from the first layer to the third layer is deepened in turn.
- the powder 3 and the powder 4 in Table 1 three kinds of composite resin material precursor powders were prepared. Then, the powder 4 is added to the mold as the first layer, after the flattening, the powder 3 is added, and the powder 3 is used as the second layer, and after flattening, the powder 1 is added, and the powder 1 is taken as the third layer. a layer in which the thickness of the powder 1 is 3 mm, the thickness of the powder 3 is 7 mm, and the thickness of the powder 4 is 4 mm, and then dry-pressed under a pressure of 10 MPa to obtain a dental material preform having a light transmittance and a color gradient. Blank body.
- the dental material preform body with light transmittance and color gradation is subjected to heat curing treatment, and the treatment temperature is 131 ° C, the pressure is 250 MPa, and the heat preservation time is 3 hours, thereby preparing a dental having three layers of light transmittance and color gradation. material.
- the chromaticity difference between the first layer and the third layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The chromaticity difference between 1 is 1 or more and 11 or less, and the chromaticity difference between the first layer and the third layer - (the chromaticity difference between the first layer and the second layer + the second layer and the third layer The difference in chromaticity)
- the light transmittance and the color gradient of the dental material prepared by using the above three powders have a light transmittance of the third layer greater than that of the second layer; the light transmittance of the second layer is greater than the transmittance of the first layer
- the color from the third layer to the first layer is deepened in turn.
- the third layer corresponds to the portion of the cut end of the tooth, and the first layer corresponds to the neck of the tooth.
- the powder 4 is added, and the powder 4 is used as the fourth layer, wherein the thickness of the powder 1 is 4 mm, the thickness of the powder 2 is 4 mm, the thickness of the powder 3 is 3 mm, and the powder 4
- the thickness of the film is 3 mm, and then dry-pressed under a pressure of 20 MPa to obtain a dental material preform having a light transmittance and a color gradient.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 185 ° C, a pressure of 300 MPa, and a holding time of 4 hours, thereby preparing a four-layer light transmittance and a color gradation.
- Dental materials are subjected to heat curing treatment at a treatment temperature of 185 ° C, a pressure of 300 MPa, and a holding time of 4 hours, thereby preparing a four-layer light transmittance and a color gradation.
- the chromaticity difference between the first layer and the third layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The difference in chromaticity is 1 or more and 11 or less, and the chromaticity difference between the third layer and the fourth layer is 1 or more and 11 or less; and
- the light transmittance and color grading dental material prepared by the above four kinds of powders have a light transmittance of the first layer greater than that of the second layer; the light transmittance of the second layer is greater than the light transmittance of the third layer; The light transmittance of the third layer is greater than the light transmittance of the fourth layer, and the color from the first layer to the fourth layer is sequentially deepened.
- the first layer corresponds to the cut end of the tooth and the fourth layer corresponds to the neck of the tooth.
- dental materials having light transmittance and color gradation can also be obtained by the method as shown in Examples 4-6.
- the four molds of 1#-4# are used, the four molds have the same shape, and the 4# mold volume>3# mold volume>2# mold volume>1# mold volume .
- the powder 4 is placed in a 1# mold, and dry pressing is performed under a pressure of 4 MPa to obtain a first green body; then the powder 2 is placed in a 2# mold, and the first green body is placed in 2#.
- the powder 2 is wrapped with the first body while the first body is located in the middle of the powder 2, and is dry-formed under a pressure of 4 MPa to obtain a second body; then the powder 1 is placed in 4
- the second blank is placed in the 4# mold, so that the powder 1 wraps the second green body while the second green body is located in the middle of the powder 1, and is dry-formed under a pressure of 4 MPa.
- Dental material preforms with light transmittance and color gradation.
- the dental material preform of the light transmittance and the color gradation is thermally cured at a treatment temperature of 115 ° C, a pressure of 160 MPa, and a holding time of 0.5 h, thereby preparing a three-layer light transmittance and a color gradient.
- Dental materials are thermally cured at a treatment temperature of 115 ° C, a pressure of 160 MPa, and a holding time of 0.5 h, thereby preparing a three-layer light transmittance and a color gradient.
- the powder 1 is the outermost layer
- the powder 2 is the outer layer
- the powder 4 is the innermost layer, wherein the outermost layer and the innermost layer.
- the chromaticity difference between the layers is 2 or more and 15 or less; the chromaticity difference between the outermost layer and the second outer layer is 1 or more and 11 or less; the chromaticity difference between the sub-outer layer and the innermost layer is 1 or more And 11 or less, and the chromaticity difference between the outermost layer and the innermost layer - (the difference in chromaticity between the outermost layer and the outer layer + the difference in chromaticity between the outer layer and the innermost layer)
- the light transmittance and the color-graded dental material prepared in Example 4 of the present application have a light transmittance decreasing from the outermost layer to the innermost layer in turn; the color is sequentially deepened from the outermost layer to the innermost layer.
- the powder 3 and the powder 4 in Table 1 three kinds of composite resin material precursor powders were prepared.
- the powder 4 is placed in a 1# mold, and dry pressing is performed under a pressure of 10 MPa to obtain a first green body; then the powder 3 is placed in a 3# mold, and the first green body is placed in a 3# mold.
- the powder 3 is wrapped in the first body while the first body is located in the middle of the powder 3, and is dry-formed under a pressure of 10 MPa to obtain a second body, and then the powder 1 is placed in 4#.
- the second blank is placed in the 4# mold, so that the powder 1 wraps the second blank while the second blank is located in the middle of the powder 1, and is dry-formed under a pressure of 10 MPa.
- Dental material preforms with light rate and color gradients.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 131 ° C, a pressure of 250 MPa, and a holding time of 3 h, thereby preparing a three-layer light transmittance and a color gradation.
- Dental materials are subjected to heat curing treatment at a treatment temperature of 131 ° C, a pressure of 250 MPa, and a holding time of 3 h, thereby preparing a three-layer light transmittance and a color gradation.
- the powder 1 serves as the outermost layer
- the powder 3 serves as the outer layer
- the powder 4 serves as the innermost layer
- the outermost layer and the innermost layer
- the chromaticity difference between the layers is 2 or more and 15 or less
- the chromaticity difference between the outermost layer and the second outer layer is 1 or more and 11 or less
- the chromaticity difference between the sub-outer layer and the innermost layer is 1 or more And 11 or less
- the light transmittance is sequentially decreased from the outermost layer to the innermost layer; the color is sequentially deepened from the outermost layer to the innermost layer.
- the powder 3 is wrapped in the first body while the first body is located in the middle of the powder 3, and is dry-formed under a pressure of 20 MPa to obtain a second body; then the powder 2 is placed in the 3# In the mold, the second blank is placed in the 3# mold, so that the powder 2 wraps the second blank while the second blank is located in the middle of the powder 2, and is dry-formed under a pressure of 20 MPa to obtain the first Three blanks, then the powder 1 is placed in the 4# mold, and the third blank is placed in the 4# mold, so that the powder 1 wraps the third blank while the third blank is located in the middle of the powder 1. Dry press molding was carried out under a pressure of 20 MPa to obtain a dental material preform body having a light transmittance and a color gradient.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 185 ° C, a pressure of 300 MPa, and a holding time of 4 h, thereby preparing a four-layer light transmittance and a color gradient.
- Dental materials are subjected to heat curing treatment at a treatment temperature of 185 ° C, a pressure of 300 MPa, and a holding time of 4 h, thereby preparing a four-layer light transmittance and a color gradient.
- the material after curing of the powder 1 can be referred to as a first layer, and similarly, the material obtained by curing the powder 2 is referred to as a second layer; the material obtained by curing the powder 3 is referred to as a third layer; The cured material is called the fourth layer.
- the chromaticity difference between the first layer and the fourth layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The difference in chromaticity is 1 or more and 11 or less; the chromaticity difference between the third layer and the fourth layer is 1 or more and 11 or less, and
- the light transmittance and color grading dental material prepared in Embodiment 6 of the present application have a light transmittance decreasing from the outermost layer to the innermost layer, that is, the light transmittance of the first layer is greater than the light transmittance of the second layer;
- the light transmittance of the second layer is greater than the light transmittance of the third layer; and
- the light transmittance of the third layer is greater than the light transmittance of the fourth layer, and the color thereof is sequentially deepened from the outermost layer to the innermost layer.
- Comparative Example 7 differs from Example 1 in that the heat curing pressure was 13 MPa, and the formulation of Comparative Example 7 and various process parameters were identical to those of Example 1.
- Comparative Example 8 differs from Example 2 in that the heat curing pressure was 16 MPa, and the formulation of Comparative Example 8 and various process parameters were identical to those of Example 2.
- Comparative Example 9 differs from Example 3 in that the heat curing pressure was 20 MPa, and the formulation of Comparative Example 9 and various process parameters were identical to those of Example 3.
- Comparative Example 10 differs from Example 4 in that the heat curing pressure was 130 MPa, and the formulation of Comparative Example 10 and various process parameters were identical to those of Example 4.
- Comparative Example 11 differs from Example 5 in that the heat curing pressure was 150 MPa, and the formulation of Comparative Example 11 and various process parameters were identical to those of Example 5.
- test method for flexural strength refers to the standard YY/T 0710-2009/ISO 10477-2004; the test method for compressive strength refers to the ISO 4049:2009 standard; the test method for fracture toughness refers to the ISO6872-2015 standard.
- Table 3 shows the properties of the dental materials prepared in Examples 1-6 and Comparative Examples 7-12.
- the flexural strength of Examples 1-3 with respect to Comparative Examples 7-9 increased from less than 213 MPa to more than 248 MPa; the compressive strength increased from 557 MPa to over 581 MPa; the fracture toughness increased from 1.3 MPa to 1.67. More than MPa.
- the flexural strength, compressive strength and fracture toughness of the light transmittance and color grading dental materials prepared by using the examples of the present application are greatly improved, thereby improving the wear resistance of the material.
- the flexural strength of Examples 4-6 with respect to Comparative Examples 10-11 was increased from less than 223 MPa to more than 252 MPa; the compressive strength was increased from 566 MPa to over 593 MPa; and the fracture toughness was increased from 1.58 MPa to 1.76 MPa or more.
- the flexural strength, compressive strength and fracture toughness of the light transmittance and color grading dental materials prepared by using the examples of the present application are greatly improved, thereby improving the wear resistance of the material.
- the weight ratio of the filler to the resin monomer is 31:69-69:31, preferably 43:57-62:38, and the weight of the initiator is a resin single. 0.1 to 3% by weight, preferably 0.1 to 2% by weight, the weight of the colorant is 0.001 to 0.2% by weight based on the total weight of the resin monomer and the filler, preferably 0.002 to 0.1%; and the pressure for dry compression molding is 11 to 19 MPa, preferably
- the heat curing treatment condition is a temperature of 151-169 ° C, preferably 155-165 ° C, a pressure of 210-300 MPa, preferably 240-290 MPa, and a holding time of 1.1-1.8 h, preferably 1.6. -1.8h.
- Table 4 shows the formulation and process parameters of four kinds of composite resin material precursor powders with different light transmittance.
- the values corresponding to the resin monomer, filler, initiator and colorant in Table 4 are parts by weight, and each part by weight may be 100 g.
- Table 5 shows the chromaticity values and light transmittance of the powders 5-8 based on the Lab color system.
- the chromaticity values and the light transmittances of the powders 5-8 are shown in Table 5.
- the light transmittance of the powders 5-8 is sequentially decreased, wherein the chromaticity of the powders 5-8 is Based on the Lab color system, the above powder is solidified under a preset condition and measured by a color difference meter or a spectrophotometer.
- the light transmittance is measured by a light transmittance tester after the powder is cured under a predetermined condition and the test light wavelength is 550 nm.
- three different colors of powder 5, powder 6 and powder 8 can be prepared by mixing the raw materials. Then, the powder 5 is added to the mold as the first layer, after the flattening, the powder 6 is added, and the powder 6 is used as the second layer, and after flattening, the powder 8 is added, and the powder 8 is taken as the third layer. a layer in which the thickness of the powder 5 is 4 mm, the thickness of the powder 6 is 6 mm, and the thickness of the powder 8 is 4 mm, and then dry-pressed under a pressure of 11 MPa to obtain a dental material preform having a light transmittance and a color gradient.
- the treatment temperature is 155 ° C
- the pressure is 210 MPa
- the holding time is 1.1 h, which can be prepared with three layers of light transmittance and color.
- Gradient dental material
- the chromaticity difference between the first layer and the third layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The chromaticity difference between 1 is 1 or more and 11 or less, and the chromaticity difference between the first layer and the third layer - (the chromaticity difference between the first layer and the second layer + the second layer and the third layer The difference in chromaticity)
- the light transmittance and the color gradient of the dental material prepared by using the above three powders have a light transmittance of the first layer greater than that of the second layer; the light transmittance of the second layer is greater than the transmittance of the third layer The color gradually deepens from the first layer to the third layer.
- the first layer corresponds to the portion of the cut end of the tooth
- the third layer corresponds to the neck of the tooth.
- the powder 7 and the powder 8 in Table 4 three kinds of composite resin material precursor powders were prepared. Then, the powder 8 is added to the mold as the first layer, after the flattening, the powder 7 is added, and the powder 7 is used as the second layer, and after flattening, the powder 5 is added, and the powder 5 is taken as the third layer. a layer in which the thickness of the powder 5 is 3 mm, the thickness of the powder 7 is 7 mm, and the thickness of the powder 8 is 4 mm, and then dry-pressed under a pressure of 16 MPa to obtain a dental material preform having a light transmittance and a color gradient. Blank body.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 165 ° C, a pressure of 240 MPa, and a holding time of 1.6 h, thereby preparing a three-layer light transmittance and a color gradient.
- Dental materials are subjected to heat curing treatment at a treatment temperature of 165 ° C, a pressure of 240 MPa, and a holding time of 1.6 h, thereby preparing a three-layer light transmittance and a color gradient.
- the chromaticity difference between the first layer and the third layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The chromaticity difference between 1 is 1 or more and 11 or less, and the chromaticity difference between the first layer and the third layer - (the chromaticity difference between the first layer and the second layer + the second layer and the third layer The difference in chromaticity)
- the light transmittance and the color gradient of the dental material prepared by using the above three powders have a transmittance of the third layer greater than that of the second layer; the transmittance of the second layer is greater than the transmittance of the first layer From the third layer to the first layer, the color gradually deepens.
- the third layer corresponds to the portion of the cut end of the tooth, and the first layer corresponds to the neck of the tooth.
- Powder 5 is added to the mold as the first layer, after the flattening, powder 6 is added, and powder 6 is used as the second layer, after flattening, powder 7 is added, and powder 7 is used as the third layer.
- the powder 8 is added, and the powder 8 is used as the fourth layer, wherein the thickness of the powder 5 is 4 mm, the thickness of the powder 6 is 4 mm, the thickness of the powder 7 is 3 mm, and the powder 8 is The thickness was 3 mm and then dry-pressed under a pressure of 19 MPa to obtain a dental material preform having a light transmittance and a color gradient.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 169 ° C, a pressure of 290 MPa, and a holding time of 1.8 h, thereby preparing a four-layer translucent transmittance and Dental material with a gradient of color.
- the chromaticity difference between the first layer and the third layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The difference in chromaticity is 1 or more and 11 or less, and the chromaticity difference between the third layer and the fourth layer is 1 or more and 11 or less; and
- the light transmittance and the color gradient of the dental material prepared by using the above four powders the light transmittance of the first layer is greater than the light transmittance of the second layer; the light transmittance of the second layer is greater than the light transmittance of the third layer; The transmittance of the third layer is greater than the transmittance of the fourth layer, and the color from the first layer to the fourth layer is gradually deepened.
- the first layer corresponds to the portion of the cut end of the tooth and the fourth layer corresponds to the neck of the tooth.
- dental materials having light transmittance and color gradation can also be obtained by the method as shown in Examples 15-17.
- the powder 6 and the powder 8 in Table 4 three kinds of composite resin material precursor powders were prepared.
- the powder 8 is placed in a 1# mold, and dry pressing is performed under a pressure of 11 MPa to obtain a first green body; then the powder 6 is placed in a 2# mold, and the first green body is placed in 2#.
- the powder 6 is wrapped around the first body while the first body is located in the middle of the powder 6, and is dry-formed under a pressure of 11 MPa to obtain a second body; then the powder 5 is placed in 4
- the second blank is placed in the 4# mold, and the powder 5 is wrapped around the second green body while the second green body is placed in the middle of the powder 5, and dry pressing is performed under a pressure of 11 MPa.
- Dental material preforms with light transmittance and color gradation.
- the dental material preform of the light transmittance and the color gradation is thermally cured at a treatment temperature of 155 ° C, a pressure of 210 MPa, and a holding time of 1.1 h, thereby preparing a three-layer light transmittance and a color gradient.
- Dental materials are thermally cured at a treatment temperature of 155 ° C, a pressure of 210 MPa, and a holding time of 1.1 h, thereby preparing a three-layer light transmittance and a color gradient.
- the powder 5 serves as the outermost layer
- the powder 6 serves as the outer layer
- the powder 8 serves as the innermost layer, wherein the outermost layer and the innermost layer
- the chromaticity difference between the layers is 2 or more and 15 or less
- the chromaticity difference between the outermost layer and the second outer layer is 1 or more and 11 or less
- the chromaticity difference between the sub-outer layer and the innermost layer is 1 or more And 11 or less
- the chromaticity difference between the outermost layer and the innermost layer - (the difference in chromaticity between the outermost layer and the outer layer + the difference in chromaticity between the outer layer and the innermost layer)
- the light transmittance and color grading dental materials prepared in Example 15 of the present application the light transmittance is sequentially decreased from the outermost layer to the innermost layer; the color is sequentially deepened from the outermost layer to the innermost layer.
- the powder 7 and the powder 8 in Table 4 three kinds of composite resin material precursor powders were prepared.
- the powder 8 is placed in a 1# mold, and dry press molding is performed under a pressure of 11 MPa to obtain a first green body; then the powder 7 is placed in a 3# mold, and the first green body is placed in a 3# mold.
- the powder 7 is wrapped in the first body while the first body is located in the middle of the powder 7, and is dry-formed under a pressure of 11 MPa to obtain a second body, and then the powder 5 is placed in 4#.
- the second blank is placed in the 4# mold, so that the powder 5 wraps the second blank while the second blank is located in the middle of the powder 5, and is dry-formed under a pressure of 11 MPa.
- Dental material preforms with light rate and color gradients.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 165 ° C, a pressure of 240 MPa, and a holding time of 1.6 h, thereby preparing a three-layer light transmittance and a color gradient.
- Dental materials are subjected to heat curing treatment at a treatment temperature of 165 ° C, a pressure of 240 MPa, and a holding time of 1.6 h, thereby preparing a three-layer light transmittance and a color gradient.
- the powder 5 serves as the outermost layer
- the powder 7 serves as the outer layer
- the powder 8 serves as the innermost layer
- the outermost layer and the innermost layer The chromaticity difference between the layers is 2 or more and 15 or less; the chromaticity difference between the outermost layer and the second outer layer is 1 or more and 11 or less; the chromaticity difference between the sub-outer layer and the innermost layer is 1 or more And 11 or less, and the chromaticity difference between the outermost layer and the innermost layer - (the difference in chromaticity between the outermost layer and the outer layer + the difference in chromaticity between the outer layer and the innermost layer)
- the light transmittance is sequentially decreased from the outermost layer to the innermost layer; the color is sequentially deepened from the outermost layer to the innermost layer.
- the powder 8 is dry-formed in a 1# mold under a pressure of 11 MPa to obtain a first green body; then the powder 7 is placed in a 2# mold, and the first green body is placed in a 2# mold. , the powder 7 is wrapped in the first body while the first body is located in the middle of the powder 7, and is dry-formed under a pressure of 11 MPa to obtain a second body; then the powder 6 is placed in the 3# mold.
- the second blank is placed in the 3# mold, so that the powder 6 wraps the second blank while the second blank is located in the middle of the powder 6, and is dry-formed under a pressure of 11 MPa to obtain a third
- the green body, the powder 5 is placed in the 4# mold, and the third blank is placed in the 4# mold, so that the powder 5 wraps the third blank while the third blank is located in the middle of the powder 5.
- Dry press molding was carried out under a pressure of 11 MPa to obtain a dental material preform having a light transmittance and a color gradation.
- the dental material preform body having the light transmittance and the color gradation is subjected to heat curing treatment at a treatment temperature of 169 ° C, a pressure of 290 MPa, and a holding time of 1.8 h, thereby preparing four layers of light transmittance and color. Gradient dental material.
- the material after the powder 5 is solidified may be referred to as a first layer, and similarly, the material obtained by curing the powder 6 is referred to as a second layer; the material obtained by curing the powder 7 is referred to as a third layer; The cured material is called the fourth layer.
- the chromaticity difference between the first layer and the fourth layer is 2 or more and 15 or less; the chromaticity difference between the first layer and the second layer is 1 or more and 11 or less; the second layer and the third layer The difference in chromaticity is 1 or more and 11 or less; the chromaticity difference between the third layer and the fourth layer is 1 or more and 11 or less, and
- the light transmittance and color grading dental material prepared in the embodiment 17 of the present application is sequentially decreased from the outermost layer to the innermost layer, that is, the light transmittance of the first layer is greater than the light transmittance of the second layer;
- the light transmittance of the second layer is greater than the light transmittance of the third layer;
- the light transmittance of the third layer is greater than the light transmittance of the fourth layer; the color is sequentially deepened from the outermost layer to the innermost layer.
- Comparative Example 18 differs from Example 12 in that the heat curing pressure was 13 MPa, and the formulation of Comparative Example 18 and various process parameters were identical to those of Example 12.
- Comparative Example 19 differs from Example 13 in that the heat curing pressure was 16 MPa, and the formulation of Comparative Example 19 and various process parameters were identical to those of Example 13.
- Comparative Example 20 differs from Example 14 in that the heat curing pressure was 20 MPa, and the formulation of Comparative Example 20 and various process parameters were identical to those of Example 14.
- Comparative Example 21 differs from Example 15 in that the heat curing pressure was 130 MPa, and the formulation of Comparative Example 21 and various process parameters were identical to those of Example 15.
- Comparative Example 22 differs from Example 16 in that the heat curing pressure was 150 MPa, and the formulation of Comparative Example 22 and various process parameters were identical to those of Example 16.
- test method for flexural strength refers to the standard YY/T 0710-2009/ISO 10477-2004; the test method for compressive strength refers to the ISO 4049:2009 standard; the test method for fracture toughness refers to the ISO6872-2015 standard.
- Table 6 shows the properties of light transmittance and color graded dental materials prepared in Examples 12-17 and Comparative Examples 18-22.
- the flexural strength of Examples 12-14 relative to Comparative Examples 18-20 increased from less than 218 MPa to more than 250 MPa; the compressive strength increased from 549 MPa to over 591 MPa; and the fracture toughness increased from 1.28 MPa to 1.72. More than MPa.
- the flexural strength, compressive strength and fracture toughness of the light transmittance and color grading dental materials prepared by using the examples of the present application are greatly improved, thereby improving the wear resistance of the material.
- the flexural strength of Examples 15-17 relative to Comparative Examples 21-22 increased from less than 220 MPa to more than 257 MPa; the compressive strength increased from 553 MPa to over 596 MPa; and the fracture toughness increased from 1.35 MPa to 1.78 MPa or more.
- the flexural strength, compressive strength and fracture toughness of the light transmittance and color grading dental materials prepared by using the examples of the present application are greatly improved, thereby improving the wear resistance of the material.
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Abstract
Description
Claims (14)
- 透光率和颜色渐变的牙科材料的制备方法,其特征在于,所述方法包括:(1)、制备至少三种不同透光率的复合树脂材料前驱粉体,其中,每一种透光率的复合树脂材料前驱粉体的制备过程包括:称取原料,所述原料包括树脂单体、填料、引发剂及着色剂,将原料混合后得到复合树脂材料前驱粉体,其中,填料与树脂单体的重量比为10:90-90:10,优选为70:30-85:15,引发剂重量为树脂单体重量的0.1-3%,优选为0.1-2%,着色剂重量为树脂单体和填料总重量的0.001-0.2%,优选为0.002-0.1%;所述树脂单体包括烯键式不饱和单体和\或环氧树脂;(2)、按照透光率从低到高的顺序,或从高到低的顺序,依次将所述至少三种不同透光率的复合树脂材料前驱粉体加入到模具中,在3-20MPa,优选为4-10MPa的压力下,干压成型,得到透光率和颜色渐变的牙科材料预成型坯体;其中,在将每一种复合树脂材料前驱粉体加入到模具中后,将该前驱粉体的上表面平整至平坦;或(2′),将所述至少三种不同透光率的复合树脂材料前驱粉体中,第一种透光率复合树脂材料前驱粉体在3-20MPa,优选为4-10MPa的压力下干压成型,得到第一坯体;将所述第一坯体包裹于所述至少三种不同透光率的复合树脂材料前驱粉体中的第二种透光率复合树脂材料前驱粉体中,在3-20MPa,优选为4-10MPa的压力下干压成型,得到第二坯体;重复进行包裹、干压成型操作,直至将所述至少三种透光率复合树脂材料前驱粉体干压成型后,得到透光率和颜色渐变的牙科材料预成型坯体,其中,所述透光率和颜色渐变的牙科材料预成型坯体中各层前驱粉体从内到外的透光率依次升高;(3)、将步骤(2)或者步骤(2′)所制备的透光率和颜色渐变的牙科材料预成型坯体进行热固化处理,得到透光率和颜色渐变的牙科材料,其中,热固化处理条件为,温度为115-185℃,优选为131-171℃,压力为大于160MPa,优选为160-300MPa,更优选为200-250MPa,保温时间为0.5-4h,优选为0.5-3 h。
- 根据权利要求1所述的方法,其特征在于,所述透光率和颜色渐变的牙科材料还具有多层色,相邻两层的复合树脂材料之间,基于Lab表色系的色度差大于等于1,且小于等于11;所述透光率和颜色渐变的牙科材料中不相邻各层的复合树脂材料之间,基于Lab表色系的色度差的最大值大于等于2,且小于等于15;所述透光率和颜色渐变的牙科材料中所有相邻各层复合树脂材料之间的色度差之和,与所述透光率和颜色渐变的牙科材料中色度值最高的一层复合树脂材料与色度值最低的一层复合树脂材料之间的色度差之差不大于2;其中,
- 根据权利要求1所述的方法,其特征在于,所述透光率和颜色渐变的牙科材料还具有多层透光率,相邻两层的透光率和颜色渐变的牙科材料之间的透光率的差为0.5-10%;不相邻两层复合树脂材料之间的透光率的差为1-15%;且透光率最高的一层复合树脂材料的可见光(波长为550nm)透光率为50-75%,透光率最低的一层复合树脂材料的透光率为30-60%,所述透光率最高的一层复合树脂材料与所述透光率最低的一层复合树脂材料之间的其他各层复合树脂材料的透光率为40-70%。
- 根据权利要求1所述的方法,其特征在于,所述填料与树脂单体的重量比为31:69-69:31,优选为43:57-62:38,引发剂重量为树脂单体重量的0.1-3%,优选为0.1-2%,着色剂重量为树脂单体和填料总重量的0.001-0.2%,优选为0.002-0.1%;所述热固化处理条件为,温度为151-169℃,优选为155-165℃,压力为210-300MPa,优选为240-290MPa,保温时间为1.1-1.8h,优选为1.6-1.8h。
- 根据权利要求1所述的方法,其特征在于,所述将原料混合后得到复合树脂材料前驱粉体,包括:将原料与球磨助剂混合,利用球磨法制备复合树脂材料前驱粉体,其中,原料:研磨球:球磨助剂的质量比为(1:1:1)-(3:6:2),优选为2:4:1,球磨时间为0.5-2h。
- 根据权利要求1所述的方法,其特征在于,所述填料的粒度范围为不大于2.5μm,优选为不大于2μm,更优选为0.05-2μm;所述填料的折射率为1.40-1.7,优选为1.45-1.6。
- 根据权利要求1所述的方法,其特征在于,所述原料还包括阻聚剂,所述阻聚剂占所述树脂单体总重量的0.1-3%,优选为0.2-2%。
- 根据权利要求1所述的方法,其特征在于,所述原料还包括促进剂,所述促进剂占所述树脂单体总重量的0.1-3%,优选为0.2-2%。
- 根据权利要求1所述的方法,其特征在于,所述原料还包括赋予荧光的试剂、指示剂、抑制剂、加速剂、粘度调节剂、润湿剂、抗氧化剂、表面活性剂、稳定剂及稀释剂中的至少一种。
- 根据权利要求1所述的方法,其特征在于,所述填料还包括纳米粒子,其中,所述纳米粒子占所述填料重量的1-25%,优选为1-15%;所述纳米粒子的平均直径为35-100nm,优选为40-50nm。
- 根据权利要求1所述的方法,其特征在于,所述原料还包括增强纤维,所述增强纤维为所述填料重量的1-30%,优选为1-10%;所述增强纤维的直径为0.1-25μm,优选为0.5-10μm;所述增强纤维的长度为0.001-1mm,优选为0.1-0.5mm;所述增强纤维的折射率为1.4-1.7,优选为1.45-1.6;所述增强纤维包含玻璃纤维、石英纤维、硅质纤维、陶瓷纤维及聚合物纤维中的一种或其组合,所述聚合物纤维优选为聚乙烯纤维。
- 根据权利要求11所述的方法,其特征在于,所述将原料混合后得到复合树脂材料前驱粉体,包括:将除增强纤维以外的树脂单体、填料、引发剂及着色剂混合后进行球磨 混料,得到原料混合物,其中,原料:研磨球:球磨助剂的质量比为(1:1:1)-(3:6:2),优选为2:4:1,球磨时间为0.5-2h;将所述原料混合物与所述增强纤维混合,得到复合树脂材料前驱粉体。
- 根据权利要求1所述的方法,其特征在于,所述着色剂包含红色着色剂、黄色着色剂及黑色着色剂中的一种或其组合,其中,所述红色着色剂占所述原料重量的0.001-0.06%,优选为氧化铁红;所述黄色着色剂占所述原料重量的0.001-0.04%,包含氧化铁黄、铋黄、钒锆黄及铈镨黄中的一种或其组合;所述黑色着色剂占所述原料重量的0-0.03%,优选为氧化铁黑。
- 根据权利要求1-13任一项所述的方法制备的透光率和颜色渐变的牙科材料。
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AU2018340731A AU2018340731B2 (en) | 2017-09-30 | 2018-05-16 | Preparation method for dental material with transmittance and color gradients and product prepared thereby |
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JP2020517809A JP6953626B2 (ja) | 2017-09-30 | 2018-05-16 | 透過率と色の勾配を有する歯科材料の調製方法及び本方法により調製される製品 |
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KR102108123B1 (ko) * | 2017-12-28 | 2020-05-07 | (주) 베리콤 | 치과용 컴포지트 블랭크 및 그의 제조방법 |
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KR20230145781A (ko) * | 2022-04-11 | 2023-10-18 | 오스템임플란트 주식회사 | 광중합형 치과용 고분자 수복재 조성물 |
CN115463038A (zh) * | 2022-08-10 | 2022-12-13 | 深圳玉汝成口腔材料有限公司 | 一种复合树脂义齿瓷块、制备方法及复合树脂义齿 |
CN115350335B (zh) * | 2022-08-16 | 2023-08-01 | 爱迪特(秦皇岛)科技股份有限公司 | 一种牙科修复用仿生复合材料及其应用 |
CN115919659A (zh) * | 2022-11-21 | 2023-04-07 | 深圳爱尔创口腔技术有限公司 | 一种含润瓷树脂的齿科修复材料及其制备方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4440878A (en) * | 1979-04-11 | 1984-04-03 | Kanebo, Ltd. | Resin-forming material, implant material and compositions for restorative material suitable for medical or dental use |
CN101244013A (zh) * | 2008-03-21 | 2008-08-20 | 华南理工大学 | 用于数控加工成型的纳米复合树脂牙科材料及其制备方法 |
CN101518499A (zh) * | 2009-04-01 | 2009-09-02 | 北京理工大学 | 以单晶金刚石为填料的口腔用光固化复合树脂及制备方法 |
CN105362084A (zh) | 2015-11-12 | 2016-03-02 | 深圳爱尔创口腔技术有限公司 | 一种牙科用多层色复合材料及其制备方法 |
CN107537061A (zh) * | 2016-06-23 | 2018-01-05 | 辽宁爱尔创生物材料有限公司 | 一种牙科用复合树脂材料的制备方法及其制备的产品 |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10323353A (ja) | 1997-05-26 | 1998-12-08 | G C:Kk | 歯科用レジン材料及びその作製方法 |
JP2004035332A (ja) * | 2002-07-03 | 2004-02-05 | Advance Co Ltd | セラミックスブロック |
DE102004017124B4 (de) * | 2004-04-07 | 2008-07-10 | Ivoclar Vivadent Ag | Härtbare Dentalmaterialien mit einer einstellbaren Transluzenz und hohen Opaleszenz |
FR2967568B1 (fr) * | 2010-11-19 | 2013-11-08 | Michael Sadoun | Procede de fabrication d'une prothese dentaire |
CN102285795A (zh) * | 2011-05-30 | 2011-12-21 | 北京大学口腔医学院 | 牙科复色可切削氧化锆陶瓷及制备方法 |
CN102344285B (zh) * | 2011-07-04 | 2013-04-17 | 辽宁爱尔创生物材料有限公司 | 改变牙科氧化锆材料透光性的方法 |
CN102228408B (zh) * | 2011-07-04 | 2013-03-06 | 辽宁爱尔创生物材料有限公司 | 牙科用透光性渐变氧化锆材料及制备工艺 |
CN102579148A (zh) * | 2012-03-05 | 2012-07-18 | 深圳市爱尔创科技有限公司 | 美学全氧化锆修复体的制备方法 |
BR112016007358A2 (pt) * | 2013-10-04 | 2017-08-01 | 3M Innovative Properties Co | bloco bruto para usinagem de próteses dentárias |
-
2017
- 2017-09-30 CN CN201710923133.XA patent/CN109589270B/zh active Active
-
2018
- 2018-05-16 AU AU2018340731A patent/AU2018340731B2/en active Active
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4440878A (en) * | 1979-04-11 | 1984-04-03 | Kanebo, Ltd. | Resin-forming material, implant material and compositions for restorative material suitable for medical or dental use |
CN101244013A (zh) * | 2008-03-21 | 2008-08-20 | 华南理工大学 | 用于数控加工成型的纳米复合树脂牙科材料及其制备方法 |
CN101518499A (zh) * | 2009-04-01 | 2009-09-02 | 北京理工大学 | 以单晶金刚石为填料的口腔用光固化复合树脂及制备方法 |
CN105362084A (zh) | 2015-11-12 | 2016-03-02 | 深圳爱尔创口腔技术有限公司 | 一种牙科用多层色复合材料及其制备方法 |
CN107537061A (zh) * | 2016-06-23 | 2018-01-05 | 辽宁爱尔创生物材料有限公司 | 一种牙科用复合树脂材料的制备方法及其制备的产品 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022092193A1 (ja) * | 2020-10-28 | 2022-05-05 | クラレノリタケデンタル株式会社 | 良好な色調適合性を有する歯科用硬化性組成物 |
CN116367806A (zh) * | 2020-10-28 | 2023-06-30 | 可乐丽则武齿科株式会社 | 具有良好的色调适应性的齿科用固化性组合物 |
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CN109589270A (zh) | 2019-04-09 |
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JP6953626B2 (ja) | 2021-10-27 |
CN109589270B (zh) | 2020-10-20 |
EP3689322C0 (en) | 2023-07-19 |
JP2020536061A (ja) | 2020-12-10 |
AU2018340731B2 (en) | 2021-05-13 |
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EP3689322A1 (en) | 2020-08-05 |
EP3689322A4 (en) | 2020-10-21 |
US11517507B2 (en) | 2022-12-06 |
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US20200268616A1 (en) | 2020-08-27 |
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