CN105708713B - A kind of dental fissure sealant and preparation method thereof - Google Patents
A kind of dental fissure sealant and preparation method thereof Download PDFInfo
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- CN105708713B CN105708713B CN201610141807.6A CN201610141807A CN105708713B CN 105708713 B CN105708713 B CN 105708713B CN 201610141807 A CN201610141807 A CN 201610141807A CN 105708713 B CN105708713 B CN 105708713B
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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
- A61K6/19—Self-expanding, e.g. for filling teeth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/60—Preparations for dentistry comprising organic or organo-metallic additives
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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
- A61K6/60—Preparations for dentistry comprising organic or organo-metallic additives
- A61K6/62—Photochemical radical initiators
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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
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
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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
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
- A61K6/76—Fillers comprising silicon-containing compounds
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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
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
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Abstract
The present invention relates to a kind of dental fissure sealants and preparation method thereof, belong to biomaterial for medical purpose field.This kind of dental fissure sealant includes following two substances：Filler, content is 5 50wt%, average grain diameter is 0.010 0.120 μm, and wherein filer content of the grain size more than 0.120 μm is less than 50wt%；Binder resin, content are 50 95wt%, are made of PEGUDMA, DIAUDMA, diluent and photoinitiator.The present invention is blended with nano zircite alcoholic solution with resin monomer, the method for solvent removal prepares fissure sealant, the method can be such that Nano filling disperses in resin monomer evenly, the content that Nano filling can be greatly increased in the case where not influencing product mobility, to enhance the mechanical strength (compression strength is at least 200MPa) of product, reduce polymerization shrinkage (being less than 5%).
Description
Technical field
The present invention relates to a kind of dental fissure sealants and preparation method thereof, belong to biomaterial for medical purpose field.
Background technology
The principle that fissure blockade prevents pit and fissure caries is that the nest ditch of tooth is filled and led up with high molecular material, and facing is made to become smooth
It is easy to clean, on the one hand, after fissure blockade, original bacterium has broken off the source of nutrition in nest ditch, gradually dead；On the other hand outer
The cariogenic bacterium in face cannot enter back into, to achieve the purpose that prevent pit and fissure caries.The closed material that fissure blockade uses is known as nest
Fissure seal and with certain anti-masticatory pressure, does not hinder feed with furrow bank close adhesion after solidification, and nest ditch seals
Close agent solidification after it is nontoxic, it is harmless.Sealer can generally retain for a long time.
There are mainly of two types for the fissure sealant being widely used at present, i.e., self-solidifying curing type is (after coating, at 1-2 minutes
It is interior, the effect through catalyst, material polymerizing curable) and visible light curable (it is irradiated 30 seconds by the light of certain wavelength, you can Gu
Change), the anti-caries effect difference of the two is little, from Clinical practice angle contrast, it is seen that light-cured type clinician's more convenient operation,
It is currently used fissure sealant.
At present fissure sealant major problem is that, in order to ensure that it, with good mobility, usually makes fissure blockade
Inorganic filler amount in agent reduces, but the reduction of amount of filler causes fissure sealant shrinking percentage in solidification and increases, is mechanical again
Intensity reduces.How to make the mobility that fissure sealant had not only had but also while there is low cure shrinkage and higher machinery
Intensity is always a research hotspot.
It by inorganic fillers and resinous substrates is the macromolecule compound resin mainly formed that fissure blockade agent material, which is a kind of,.
Wherein, resinous substrates are the main parts in compound resin, generally by the larger monomer of viscosity (sticky monomer) and oligomer (packet
Include performed polymer, cross-linking monomer) and the compositions such as diluent (diluting monomer).Its continuous phase as inorganic filler, in initiator
Under the action of, can curing molding in shorter time at room temperature, and assign material certain physical mechanical property and clinic
Operating characteristics.Wherein performed polymer is most important component part, is not only related to the color and luster of resin, and influence processing performance,
Physical and chemical performance.
Although general gear division fissure sealant matrix mostly uses Bis-GMA on current domestic and international market, it is right
The adhesion strength of tooth is not very big, and viscosity is high, and polymerisation conversion is low, and service life is not grown, while water resistance is poor, in mouth
Under the long term of chamber saliva, dissolving easily occurs and falls off.And it contains bisphenol-A, and bio-safety performance need further
It confirms.
It is not easy to operate since Bis-GMA viscosity is larger, it is therefore desirable to which that diluting monomer diluent improved effect is added, and it is grasped
Make performance.Diluting monomer not only plays diluent, while can also participate in reaction and be used as a kind of crosslinking agent.But at present
The shortcomings of it is short all to there is storage period in used diluent, easy to change, and polymerisation conversion is low, polymerization shrinkage is big.And at present extensively
The TEGDMA of use or a kind of comprehensive performance are preferable, are a kind of widely used diluent of producer.But its storage period still compares
The storage period of Bis-GMA resinoid monomers is short, and polymerisation conversion is low, while its adhesion strength is not also high.
Although the basic components of fissure sealant are grasped by people, ultra micro inorganic filler is equal in high viscosity monomer
Even dispersion is very difficult, and leading to fissure sealant, in solidification, shrinking percentage increases, mechanical strength reduces.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of dental fissure sealant, which is one
Kind tooth fissure blockade composition, wherein being mixed with evenly dispersed ultra-fine enhancing particle, which shows in Clinical practice
Go out high intensity, sustained release fluorine ion, good wearability, low polymerization shrinkage.
It is molten with nano zirconia alcohol it is a further object of the present invention to provide the preparation method of above-mentioned dental fissure sealant
Liquid is blended with resin monomer, solvent removal and filler prepare fissure blockade with the method that resin monomer mechanical mixture is combined
Agent, compared to only fissure sealant is prepared with inorganic filler and this conventional method of resin monomer mechanical blending, the method can make
Nano filling disperses evenly in resin monomer, and nanometer can be greatly increased in the case where not influencing product mobility and is filled out
The content of material, to enhance the mechanical strength of fissure sealant, reduce the polymerization shrinkage of fissure sealant.
To achieve the above object, the present invention uses following technical scheme：
A kind of dental fissure sealant includes following two substances by weight percentage：
Filler, content 5-50wt%, average grain diameter be 0.010-0.120 μm (0.02 μm, 0.05 μm, 0.08 μm, 0.10
μm)；In the filler, filer content of the grain size more than 0.120 μm is less than 50wt%；
Binder resin, content 50-95wt%, the binder resin are composed of the following components：Polyethylene glycol 400 is modified ammonia
Carbamate double methyl methacrylate (PEG 400Extended Urethane Dimethacrylate, abbreviation PEGUDMA),
Dimeric dibasic acid carbamate double methyl methacrylate (Dimer Acid Urethane Dimethacrylate, referred to as
DIAUDMA), diluent and photoinitiator.
Above-mentioned dental fissure sealant, as a preferred implementation manner, in the binder resin, with polyethylene glycol
400 modified urethane double methyl methacrylates (PEG 400Extended Urethane Dimethacrylate, referred to as
PEGUDMA), dimeric dibasic acid carbamate double methyl methacrylate (Dimer Acid Urethane Dimethacrylate, letter
DIAUDMA), diluent and photoinitiator be referred to as 100wt% meters, polyethylene glycol 400 modified urethane methacrylate
The content of ester and dimeric dibasic acid carbamate double methyl methacrylate is 84-99wt%；The content of diluent is 0-15wt%；Light
The content of initiator is 1.0-2.5wt%.It is highly preferred that the polyethylene glycol 400 modified urethane methacrylate
Ester (PEGUDMA) and the mass ratio of the dimeric dibasic acid carbamate double methyl methacrylate (DIAUDMA) are 0.4-2.5:1
(such as 0.5:1、0.7:1、1:1、1.5:1、2:1、2.2:1、2.4:1).The advantages of PEGUDMA is intensity height, and DIAUDMA's is excellent
Point is that polymerization shrinkage is small, and the two mass ratio is maintained above range and the two preferably cooperation advantage may be implemented.
Above-mentioned dental fissure sealant, the diluent is hydroxyethyl methacrylate second as a preferred implementation manner,
Ester (HEMA).
The present invention absorbs inventor's obtained experience in the R＆D process of light-cured composite, most using the world
Novel resin modified monomer replaces the tackifying resin monomer in present fissure sealant product, improves and is set in fissure sealant
The mobility and intensity of alicyclic monomer, reduce the polymerization shrinkage of resin monomer.Specifically the resinous substrates of the invention used are
PEGUDMA and DIAUDMA, because PEGUDMA has mechanical strength more higher than Bis-GMA, better biocompatibility and more
High polymerisation conversion；DIAUDMA has biocompatibility more better than Bis-GMA, higher polymerisation conversion and lower
Polymerization shrinkage；Additionally due to the viscosity of PEGUDMA and DIAUDMA is far below Bis-GMA, to be remarkably improved nest ditch envelope
The amount of filler of agent is closed without influencing its mobility.The present invention is used as diluent using hydroxyethyl methacrylate (HEMA), has
The advantages that storage period is long, and dilution effect is good, and adhesion strength is high can improve the adhesive property of fissure sealant.
Above-mentioned dental fissure sealant, the photoinitiator is by N, TMSDMA N dimethylamine base as a preferred implementation manner,
Ethyl methacrylate, 2,6- toluene di-tert-butyl phenols and camphorquinone composition.
Above-mentioned dental fissure sealant, as a preferred implementation manner, in the filler, 0.120 μm of grain size ＞
The percentage of filler weight and filler total weight be not higher than 10%.Because bulky grain is more, wear-resisting property is poorer, to control
The content of bulky grain processed.
Above-mentioned dental fissure sealant, as a preferred implementation manner, in the filler, grain size≤0.01 μm filler
The percentage of weight and filler total weight is 1.0-10.0%.Because while the wearability of little particle filler is good, but if small
If grain too high levels, the flexural strength of fissure sealant can be very poor；In order to realize fissure sealant wearability and flexural strength
Equilibrium, filler average grain diameter of the invention will control 0.010-0.120 μm.
Above-mentioned dental fissure sealant, the filler can be fluoride processing or untreated silica, aluminium oxide,
The inorganic particles such as alumino-silicate, titanium oxide, silanization barium aluminosilicate, the filler is fluorine as a preferred implementation manner,
The silanization barium aluminosilicate of compound processing.
Above-mentioned dental fissure sealant also contains in the dental fissure sealant as a preferred implementation manner,
There is nano zircite.Addition nano zircite can enhance the abrasion resistance of fissure sealant, so as to increase nest ditch envelope
Close the retention time of agent in the oral cavity.It is highly preferred that in the dental fissure sealant, the content of the filler is 5-
50wt%；The content of the binder resin is 35-75wt%；The content of the nano zircite is 10-22wt%.Further
The average grain diameter on ground, the nano zircite is 5-10nm (such as 6nm, 7nm, 8nm, 9nm).
A kind of preparation method of above-mentioned dental fissure sealant, specifically comprises the following steps：
The preparation process of binder resin mixes each component for forming the binder resin first, in accordance with said ratio
Processing obtains uniform binder resin；
Filling step finally obtains institute according to said ratio by the filling packing to the uniform binder resin
State dental fissure sealant.
In above-mentioned preparation method, as a preferred implementation manner, when in the dental fissure sealant also contain receive
Further include nano zircite and binder resin between the preparation process of the binder resin and the filling step when rice zirconium oxide
Mixture preparation process, be added nano zircite ethanol solution into the binder resin according to said ratio, mixing is certain
Removal alcohol solvent is finally dried in time under light protected environment, to obtain the mixing of nano zircite and binder resin
Object.It is highly preferred that in the mixture preparation process of the nano zircite and binder resin, the time of the mixing is 0.5-
1.5h (such as 0.8h, 1.2h), the temperature of the mixing are 20-30 DEG C (such as 22 DEG C, 25 DEG C, 28 DEG C), the drying be
Dry 0.5-1.5h (such as 0.8h, 1.2h) under -0.1MPa in Rotary Evaporators.Further, the nano zircite ethyl alcohol
A concentration of 15-25wt% (such as 16%, 18%, 21%, 23%, 24%) of solution.
In above-mentioned preparation method, as a preferred implementation manner, in the preparation process of the binder resin, the mixing
The time of processing is 20-40min (such as 25min, 28min, 32min, 35min, 38min), and the temperature of the mixed processing is
20-30 DEG C (such as 22 DEG C, 24 DEG C, 26 DEG C, 28 DEG C).
In above-mentioned preparation method, the filling step comprises the following specific steps that as a preferred implementation manner,：By institute
It states uniform binder resin or the nano zircite is added in mixer with the mixture of binder resin and mixes, constant temperature is extremely
40-60 DEG C (such as 42 DEG C, 45 DEG C, 48 DEG C, 52 DEG C, 55 DEG C, 58 DEG C), then according to it is above-mentioned it is corresponding proportioning by the filler in 2-
4h (such as 2.5h, 3h, 3.5h) inner edge mixing side is slowly added to；It is further continued for mixing 1-1.5h (such as 1.2h, 1.4h) and one
Determine that gained resin paste material vent is finally obtained the dental fissure sealant under vacuum degree.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) present invention has done a large amount of improvement to existing fissure sealant, including, the application of novel monomeric, special
Formula design makes the performance of material improve a lot, the present invention without the Bis-GMA or its modified monomer etc. with bisphenol-A
The compression strength for providing dental fissure sealant is at least 200MPa, and polymerization shrinkage is less than 5%.
(2) traditional mechanical agitation methods are nano particle can not to be made to be dispersed in resin monomer, nano particle group
Poly- phenomenon is very serious, and solution mixing can effectively avoid the reunion of nano particle, to make it be dispersed in
In resin.The present invention is blended with nano zircite alcoholic solution with resin monomer, the method for solvent removal prepares fissure sealant, phase
Than in preparing fissure sealant with inorganic filler and this conventional method of resin monomer mechanical blending, the method can make Nano filling
Disperse evenly, containing for Nano filling can be greatly increased in the case where not influencing product mobility in resin monomer
Amount, to enhance the mechanical strength of fissure sealant, reduce the polymerization shrinkage of fissure sealant.
(3) dental fissure sealant of the preparation method proposed by the present invention using acrylate as photo polymerization monomer,
Heat release is few, contraction is small, the degree of cross linking is high, intensity is high in entire solidification process, and the adhesive strength of material and tooth is high after solidification, and
Any unconverted monomer is not contained after solidification, be harmful to monomer so as to avoid these generates damage to tissue.
(4) dental nest ditch of the preparation method proposed by the present invention using the inorganic particle that is handled through perfluoro-compound as filler
Sealer, material can be with sustained release fluorine ion, so as to preventing decayed tooth or the effect for preventing dental caries from further destroying after solidification.This hair
The curing mechanism of polymer is photocuring in the preparation method of bright proposition, therefore is exposed under light and can accelerate to polymerize and solid
Change process.
(5) technology solves the technical barrier that clinical requirement is not achieved in domestic fissure sealant product quality, after operation
Also the situation that existing fissure sealant is completely dependent on import can be solved, cheap price must be able to be that vast oral cavity patient is universal
Receive, safe, cheap, high quality fissure blockade agent material is provided for patient；Its social benefit, economic benefit are huge.
Specific implementation mode
The technical scheme of the invention is described in detail through specific implementation examples.In embodiment, polyethylene glycol 400
Modified urethane double methyl methacrylate (400 Extended Urethane Dimethacrylate of PEG, referred to as
PEGUDMA ESSTECH companies of the U.S., dimeric dibasic acid carbamate double methyl methacrylate (Dimer Acid) are purchased from
Urethane Dimethacrylate, abbreviation DIAUDMA) ESSTECH companies of the U.S. are purchased from, diluent and photoinitiator are purchased
From SIGMA companies of the U.S.；Nano zircite ethanol solution is purchased from NYACPL NANO TECHNOLOGLE, INC., the U.S.；Fluorination
The silanization barium aluminosilicate (GM39923 Raw glass (25% barium content)) of object processing is purchased from Schott Glasswerke,
Lan Cihute, Germany.
Embodiment 1
The specific preparation method for the dental fissure sealant that embodiment 1 provides is as follows：
(1) 100g binder resins each component (in binder resin the content of each component as described in table 1) is added to a line
In planetary mixer and constant temperature is to 25 DEG C, and planetary-type mixer is started 30 minutes with compound tree lipid phase；150g is added thereto
The nano zircite ethanol solution of a concentration of 20wt% continues mixing 1 hour, and the wherein grain size of zirconium oxide is 5-10nm；Then,
Mixed solution is removed into alcohol solvent in dry 1 hour at -0.1MPa with Rotary Evaporators in light protected environment, is received
The mixture for the nano zircite and binder resin that rice zirconia content is 23%.
(2) it (is filled out with preparation test sample 1 in the mixture of 20wt% filling packings to nano zircite and binder resin
Material is 20 with the mass ratio of nano zircite and the mixture of binder resin:80), multiple with 30wt% filling packing nano zircites
Resin prepares test sample 2, and (i.e. filler and the mass ratio of nano zircite and the mixture of binder resin are 30:70) it, uses
40wt% filling packing nano zircite compound resins prepare test sample 3 (i.e. filler and nano zircite and binder resin
The mass ratio of mixture is 40:60)；3 (i.e. filler of test sample is prepared with 50wt% filling packing nano zircite compound resins
It is 50 with the mass ratio of nano zircite and the mixture of binder resin:50)；Use 3M companies CONSICE fissure sealants as
Comparative sample.Specific fill method is as follows：By the mixture of nano zircite and binder resin obtained in step (1) be added to
In planetary-type mixer and constant temperature is to 50 DEG C, then by the filler containing physical parameter and component listed in table 2 at about 3 hours
Time in be slowly added to；It is further continued for mixing 1 hour and under vacuum degree condition by the resin paste material vent of gained, finally
Obtain the dental fissure sealant.
All tests use the ISO method of standard to implement, and standard deviation is listed in bracket.Wherein, Luo Kewei
You are at the test method of hardness：In a diameter of 10mm and highly being averaged for 3 measured values on the cylindrical sample surface of 4mm
Value；By the sample photocuring 40 seconds, and placed 24 hours in 37 DEG C of water before measuring.Table 2 details the present embodiment
The physical property of obtained test sample pastes and comparative sample, as can be seen from Table 2：The present invention is total by solution
Mixed method effectively increases the addition of Nano filling under the premise of not influencing product mobility；It is tried compared to comparing
No matter sample, fissure sealant manufactured in the present embodiment greatly change in mechanical properties or have in terms of polymerization shrinkage
Into.
Binder resin forms in 1 embodiment of the present invention 1 of table
| Polyethylene glycol 400 modified urethane double methyl methacrylate | 50.2wt% |
| Dimeric dibasic acid carbamate double methyl methacrylate | 35.5wt% |
| Hydroxyethyl methacrylate | 13.0wt% |
| N, TMSDMA N dimethylamine amino ethyl methacrylate | 1.0wt% |
| 2,6- toluene di-tert-butyl phenols | 0.05wt% |
| Camphorquinone | 0.25wt% |
| It amounts to | 100 |
The physical property of fissure sealant and comparative sample prepared by 2 embodiment of the present invention 1 of table
Embodiment 2
The specific preparation method for the dental fissure sealant that embodiment 2 provides is as follows：
(1) it by 100g binder resins each component (binder resin composition is as described in table 3 in the embodiment of the present invention 2), is added
To simultaneously planetary-type mixer is started 30 minutes with compound tree lipid phase by constant temperature to 25 DEG C in a planetary-type mixer；Thereto plus
The nano zircite ethanol solution for entering 150g a concentration of 20% continues mixing 1 hour, and the wherein grain size of zirconium oxide is 5-10nm, will
Mixed solution removes alcohol solvent in dry 1 hour at -0.1MPa in light protected environment with Rotary Evaporators, obtains nanometer
The nano zircite compound resin that zirconia content is 23%.
(2) it (is filled out with preparation test sample 5 in the mixture of 25wt% filling packings to nano zircite and binder resin
Material is 25 with the mass ratio of nano zircite and the mixture of binder resin:75), multiple with 35wt% filling packing nano zircites
Resin prepares test sample 6, and (i.e. filler and the mass ratio of nano zircite and the mixture of binder resin are 35:65) it, uses
45wt% filling packing nano zircite compound resins prepare test sample 7 (i.e. filler and nano zircite and binder resin
The mass ratio of mixture is 45:55)；Comparative sample is prepared with 3M companies CONSICE fissure sealants.Nano zircite is compound
Resin is added into planetary-type mixer and constant temperature is to 50 DEG C, and the filler of component then will be admixed containing physics listed in table 4
It was slowly added within about 3 hours time；It is further continued for mixing 1 hour and under certain vacuum degree by the resin paste material of gained
Material exhaust, finally obtains the dental fissure sealant.All tests use the ISO method of standard to implement, and will mark
Quasi- deviation is listed in bracket.Wherein, the test method of rockwell's hardness is：In a diameter of 10mm and the cylinder that height is 4mm
The average value of 3 measured values of shape specimen surface；By the sample photocuring 40 seconds, and put in 37 DEG C of water before measuring
It sets 24 hours.Table 4 detail test sample pastes obtained by the present embodiment and comparative sample physical property and performance,
As can be seen from Table 4：Diluent resin can not also be added in preparation method provided by the invention, existed by the method for solution blending
The addition of Nano filling is not influenced to effectively increase under the premise of product mobility；Compared to comparative sample, the present embodiment
No matter the fissure sealant of preparation greatly improves in mechanical properties or in terms of polymerization shrinkage；Compared to adding
Enter the test sample (the test sample 1- test samples 4 in embodiment 1) of diluent, this experimental sample is in mechanical properties base
This does not change, but further reduced the polymerization shrinkage of product, to further improve the Clinical practice effect of product.
Binder resin forms in 3 embodiment of the present invention 2 of table
| Polyethylene glycol 400 modified urethane double methyl methacrylate | 60% |
| Dimeric dibasic acid carbamate double methyl methacrylate | 38.7% |
| N, TMSDMA N dimethylamine amino ethyl methacrylate | 1.0wt% |
| 2,6- toluene di-tert-butyl phenols | 0.05wt% |
| Camphorquinone | 0.25wt% |
| It amounts to | 100 |
The physical property of fissure sealant and comparative sample prepared by 4 embodiment of the present invention 2 of table
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (14)
1. a kind of dental fissure sealant, which is characterized in that include following two substances by weight percentage：
Filler, content 5-50wt%, average grain diameter are 0.010-0.120 μm；In the filler, grain size is more than 0.120 μm
Filer content be less than 50wt%；
Binder resin, content 50-95wt%, the binder resin are composed of the following components：Polyethylene glycol 400 modified amido first
Acid esters double methyl methacrylate, dimeric dibasic acid carbamate double methyl methacrylate, diluent and photoinitiator；
In the binder resin, with polyethylene glycol 400 modified urethane double methyl methacrylate, dimeric dibasic acid carbamic acid
Ester double methyl methacrylate, diluent and photoinitiator are counted for 100wt%, the double methyl of polyethylene glycol 400 modified urethane
The content of acrylate and dimeric dibasic acid carbamate double methyl methacrylate is 84-99wt%；The content of diluent is 0-
15wt%；The content of photoinitiator is 1.0-2.5wt%；The polyethylene glycol 400 modified urethane methacrylate
The mass ratio of ester and the dimeric dibasic acid carbamate double methyl methacrylate is 0.4-2.5:1.
2. dental fissure sealant according to claim 1, which is characterized in that the diluent is hydroxyethyl methacrylate second
Ester；The photoinitiator is by N, TMSDMA N dimethylamine amino ethyl methacrylate, 2,6- toluene di-tert-butyl phenols and camphorquinone composition；
The filler is fluoride processing or untreated silica, aluminium oxide, alumino-silicate, titanium oxide or silanization barium manosil AS
Salt.
3. dental fissure sealant according to claim 2, which is characterized in that the filler is the silane of fluoride processing
Change barium aluminosilicate.
4. dental fissure sealant according to claim 1, which is characterized in that in the filler, 0.120 μm of grain size ＞
The percentage of filler weight and filler total weight be not higher than 10%.
5. dental fissure sealant according to claim 1, which is characterized in that in the filler, grain size≤0.01 μm is filled out
Expect that the percentage of weight and filler total weight is 1.0-10.0%.
6. dental fissure sealant according to claim 1, which is characterized in that also contain in the dental fissure sealant
There is nano zircite.
7. dental fissure sealant according to claim 6, which is characterized in that in the dental fissure sealant,
The content of the filler is 5-50wt%, and the content of the binder resin is 35-75wt%, and the content of the nano zircite is
10-22wt%.
8. dental fissure sealant according to claim 7, which is characterized in that the average grain diameter of the nano zircite is
5-10nm。
9. the preparation method of any one of the claim 1-5 dental fissure sealants, which is characterized in that specifically include as
Lower step：
The preparation process of binder resin will form the binder resin first, in accordance with any proportionings of claim 1-5
Each component carries out mixed processing and obtains uniform binder resin；
Step is filled, according to the proportioning described in any one of claim 1-5 by the filling packing to the uniform base-material
In resin, the dental fissure sealant is finally obtained.
10. preparation method according to claim 9, which is characterized in that also contain when in the dental fissure sealant
Further include nano zircite and base-material tree between the preparation process of the binder resin and the filling step when nano zircite
Nanometer is added into the binder resin according to the proportioning described in any one of claim 6-8 in the mixture preparation process of fat
Zirconium oxide ethanol solution mixes certain time, removal alcohol solvent is finally dried under light protected environment, to obtain nanometer
The mixture of zirconium oxide and binder resin.
11. preparation method according to claim 10, which is characterized in that in the mixed of the nano zircite and binder resin
Close in object preparation process, time of the mixing is 0.5-1.5h, and the temperature of the mixing is 20-30 DEG C, the drying be
Dry 0.5-1.5h under -0.1MPa in Rotary Evaporators.
12. preparation method according to claim 11, which is characterized in that the nano zircite ethanol solution it is a concentration of
15-25wt%.
13. according to the preparation method described in any one of claim 9-12, which is characterized in that the preparation of the binder resin walks
In rapid, the time of the mixed processing is 20-40min, and the temperature of the mixed processing is 20-30 DEG C.
14. according to the preparation method described in any one of claim 9-12, which is characterized in that the filling step includes as follows
Specific steps：The uniform binder resin or the mixture of the nano zircite and binder resin are added in mixer
Mixing, constant temperature to 40-60 DEG C, then according to claim 1-8 it is any it is described proportioning by the filler on 2-4h inner edge mixing side
It is slowly added to；It is further continued for mixing 1-1.5h and under certain vacuum degree by gained resin paste material vent, finally obtains described
Dental fissure sealant.
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| CN107670112A (en) * | 2017-08-30 | 2018-02-09 | 浙江美加华医疗技术有限公司 | A kind of organic-inorganic nanocomposite corona and its 3D subtraction preparation method |
| CN108158827A (en) * | 2017-12-22 | 2018-06-15 | 黄小艳 | A kind of composite material for dental prosthetic |
| JP6533332B1 (en) * | 2018-12-06 | 2019-06-19 | Ｙａｍａｋｉｎ株式会社 | Dental adhesive composition |
| CN115212117A (en) * | 2022-07-13 | 2022-10-21 | 北京安泰生物医用材料有限公司 | Flowable dental filling resin and preparation method thereof |
| CN115381722A (en) * | 2022-09-28 | 2022-11-25 | 桂林凯文彼德科技有限公司 | Dental color-changing pit and fissure sealant, and preparation method and application thereof |
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| CN1981736A (en) * | 2005-12-15 | 2007-06-20 | 安泰科技股份有限公司 | Dental composite resin |
| CN101347386A (en) * | 2008-08-28 | 2009-01-21 | 成都军区昆明总医院 | Dentistry compound resin ceramic whisker stuffing surface modification and method of preparing the same |
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| CN1981736A (en) * | 2005-12-15 | 2007-06-20 | 安泰科技股份有限公司 | Dental composite resin |
| CN101347386A (en) * | 2008-08-28 | 2009-01-21 | 成都军区昆明总医院 | Dentistry compound resin ceramic whisker stuffing surface modification and method of preparing the same |
| CN103126908A (en) * | 2012-03-16 | 2013-06-05 | 中新棠国业（北京）科技有限责任公司 | Dental prepolymerized resin filler type composite resin |
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