CN101564357B - Photo-curing composition for tooth - Google Patents
Photo-curing composition for tooth Download PDFInfo
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- CN101564357B CN101564357B CN2009101118870A CN200910111887A CN101564357B CN 101564357 B CN101564357 B CN 101564357B CN 2009101118870 A CN2009101118870 A CN 2009101118870A CN 200910111887 A CN200910111887 A CN 200910111887A CN 101564357 B CN101564357 B CN 101564357B
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Abstract
The invention relates to a photo-curing composition for tooth, with belongs to the field of preparation for dentistry. The object of the invention is to solve the problem that the abrasion resistance and obdurability of photo-curing dentistry compound resin material for filling tooth cavity is needed to be improved urgently. The composition provided by the invention comprises the following components, in mass percentages, nano inorganic powder treated by surface modification with silicone hydride coupling agent 20-85%; resin monomer such as bisphenol A glycidyl methacrylate 8%-70%; fluidifyingagent such as triethylene glycol dimethacrylate 5%-25%; photoinitiator such as camphorquinon 0.25%-2%; coinitiator such as 2-(dimethylamino)ethyl methacrylate 0.5%-3%; the main point of the invention is the nano inorganic powder contains flaky alumina granules 10-80 wt.% based on its own weight. Flaky alumina granule component in the composition provided by the invention contributes to improve ab rasion resistance and obdurability of photo-curing material.
Description
Technical field
The present invention relates to a kind of photo-curing composition for tooth, belong to that A61K is medical, the dental preparation field.
Background technology
Still higher in view of present dental caries incidence rate, cavity is filled also has a large amount of medical applications demands with material, and the degree of depth R﹠D work of this class material has the progressive practical significance of the medical skill of promotion; Under the joint efforts of chemical material expert and dental medicine brainstrust, in recent years, generally accepted gradually as filling out the dental caries material with the photocuring dentistry compound resin material.
The photocuring dentistry compound resin material also claims visible-light curing composite resin (VLC), is that the visible light with specific wavelength and intensity comes initiated polymerization.The product in past mostly is ultraviolet light (UV) curing materials.The composite resin prescription that occurs on the current international market has kind more than 50, and they can be divided into different classifications, and has bigger difference on composition and performance.Its composition introduction of the photocuring dentistry compound resin material that manufacturer announced is more rough usually, and important data then need could obtain by chemical analysis.The basic composition of photocuring dentistry compound resin material comprises: resinous substrates, inorganic filler, polymerizing curable cause material, polymerization inhibitor and coloring agent; The effect of resinous substrates is to give plasticity, curing characteristics and intensity, resinous substrates commonly used is the polyfunctional group methacrylate monomer, the polyfunctional group methacrylate monomer relates to miscellaneous similar chemical substance, actual polyfunctional group methacrylate monomer commonly used is the selection of having taken all factors into consideration the each side factor in the dentistry compound resin material, concrete example such as BIS-GMA, UDMA and TEGDMA, BIS-GMA wherein, UDMA or their combination have viscosity higher, and TEGDMA joins BIS-GMA for reducing viscosity as diluent, in UDMA or their combination; The effect of inorganic filler is to gain in strength and wearability, inorganic filler commonly used such as silica flour, silicon dioxide powder, glass dust; The effect that polymerizing curable causes material is the trigger monomer polymerizing curable, and polymerizing curable causes material and generally includes initiator and coinitiator, and described initiator and coinitiator can be respectively camphorquinone and tertiary amine; Inhibitor action is to keep effective life, and described polymerization inhibitor mostly is phenols; The effect of coloring agent is to give the natural teeth color and luster, described coloring agent such as titanium white, chrome yellow.The dummy suffix notation BIS-GMA acute pyogenic infection of finger tip bisphenol-A glycidyl methacrylate that above relates to; Dummy suffix notation UDMA acute pyogenic infection of finger tip carbamate double methyl methacrylate; Dummy suffix notation TEGDMA acute pyogenic infection of finger tip double methyl methacrylate triethylene glycol ester; Dummy suffix notation BPO acute pyogenic infection of finger tip benzoyl peroxide, benzoyl peroxide has another name called dibenzoyl peroxide; Dummy suffix notation DHET acute pyogenic infection of finger tip N, the N-dihydroxyethyl p-toluidine.More than the Chinese of cited various related substanceses and the art-recognized meanings of English alphabet dummy suffix notation indication, for the dental profession technical staff, its art-recognized meanings is known.
In each composition of photocuring dentistry composite resin, for amorphous granular is adopted in the inorganic filler of gaining in strength and wearability adds more, the effect that it can be brought into play in composite resin is similar to spheroidal particle, surface layer at the dentistry composite resin after polyreaction is solidified, faying face between amorphous granular and the resin matrix is less, anchor force thus a little less than, in friction process, peel off easily, this factor makes amorphous granular make a discount in the effect aspect the lifting dentistry composite resin wearability, on the other hand, in the dentistry composite resin body after solidifying, the rough approximation substantially of amorphous granular is in spheric pattern, also extracts toughening mechanisms some shortcomings have been arranged because of fully not taking into account for the Strengthening and Toughening contribution of dentistry composite resin.
Extract toughening mechanisms and come the Strengthening and Toughening dentistry composite resin for utilizing fully, in recent years, the glass fibre that draw ratio is very high, silicon carbide whisker, silicon nitride crystal whisker and aluminium borate whisker etc. are as considerable inorganic filler, obtain some research staff's concern, undoubtedly, the inorganic filler that this class draw ratio is very high is if can sneak into equably in the resin, benefiting of a front will be provided the Strengthening and Toughening of photocuring dentistry composite resin, but, the glass fibre that draw ratio is very high, silicon carbide whisker, silicon nitride crystal whisker and aluminium borate whisker etc. are difficult to sneak into equably in the resin matrix because of its inherent physics pattern, in other words, uniform mixing becomes and is difficult for the obstacle gone beyond together, this factor, make the glass fibre that draw ratio is very high, silicon carbide whisker, the application of inorganic material such as silicon nitride crystal whisker and aluminium borate whisker in the photocuring dentistry composite resin can be not fully, put to good use all sidedly, about this point, in cavity is filled with photocuring dentistry compound resin material field, show particularly evidently.
Summary of the invention
Technical problem to be solved by this invention is, demand the further technical development actual requirement of raising urgently at existing photocuring dentistry composite resin anti-wear performance and toughness and tenacity, develop a kind of new photocuring dental resin composition, this photocuring dental resin composition should be taken the raising of wearability into account, also to take into account and extract toughening mechanisms the front of Strengthening and Toughening is benefited, simultaneously, in preparation, produce in the stage of this photocuring dental resin composition, should be easily and other composition uniform mixing of compositions for increasing its relevant composition of inorganic filler that wearability and obdurability add therebetween, avoid occurring described mixing obstacle.
The present invention solve the technical problem by following scheme, and this scheme provides a kind of photo-curing composition for tooth, and the weight percentage of each composition is as follows in the said composition:
Resin monomer 8%～70%;
Diluent 5%～25%;
Light trigger 0.25%～2%;
Coinitiator 0.5%～3%;
Inorganic nano-filler 20%～85% after the modification;
Wherein, the inorganic nano-filler after the described modification is to be handled through silane coupler by nano inorganic powder, and the powder body material that forms after the drying, pulverizing; It is 10%～80% flaky silicon dioxide granule that described nano inorganic powder contains the percetage by weight that accounts for nano inorganic powder weight; The particulate plate width of described flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of described flaky silicon dioxide and sheet is between 3 and 40.
The particulate plate width of described flaky silicon dioxide can be the arbitrarily selected width between 0.3 micron and 36.0 microns, and still, the preferred value of the particulate plate width of flaky silicon dioxide is between 0.3 micron and 0.9 micron.Undersized flaky silicon dioxide granule more helps married operation.
Described resin monomer comprises the low molecular weight monomers form and is so-called oligomer form by the bigger morphon of the molecular weight of low molecular weight monomers after low polymerization that the preferred value of described its molecular weight of resin monomer is between 200～5000; Described resin monomer is a polyfunctional group methyl acrylic ester material, the polyfunctional group methacrylate monomer relates to miscellaneous similar chemical substance, this class material all is easy to realize polymerizing curable between monomer fast under the initiation of polymerizing curable initiation material, described resin monomer preferred material is a kind of or both combinations in bisphenol-A glycidyl methacrylate, the carbamate double methyl methacrylate; Because above-mentioned preferred monomer is the bisphenol-A glycidyl methacrylate, class materials such as carbamate double methyl methacrylate have higher viscosity, for ease of the adding operation of inorganic nano-filler and the practical application of making finished product, diluent components is necessary in the compositions, the existence of diluent can reduce the viscosity of composite resin paste, the optional material of diluent that is suitable for this case purpose is more, and described diluent preferred material is a double methyl methacrylate triethylene glycol ester, Ethylene glycol dimethacrylate, the combination of one or more in the hydroxyethyl methylacrylate.Described diluent is participating in there is no too big-difference with materials such as described bisphenol-A glycidyl methacrylate and carbamate double methyl methacrylates aspect the cross-linking and curing reaction, distinguish with diluent one speech, be that mainly this class material is for reducing the composition that viscosity adds from function more significantly.
This case photocuring dental resin composition is applicable to that light radiation causes the application mode of curing cross-linking reaction, the preferred camphorquinone of light trigger, coinitiator preferable methyl acrylic acid diformazan ammonia ethyl ester.
Silane coupler is used for the surface modification of nano inorganic powder, commercially available silane coupler applicable to this case purpose has multiple, concrete example such as KH-550, KH-560, KH-570 etc., comprehensive many-sided factor, the KH-570 of the preferred medical grade of described silane coupler, all there is introduction in each corresponding producer of the condition of manipulating of above-mentioned various commercially available silane couplers, and the condition of manipulating of all kinds of commercially available silane couplers is known.
Above address, it is 1%～80% flaky silicon dioxide granule that the described nano inorganic powder of this case contains the percetage by weight that accounts for nano inorganic powder weight; It is other the selected arbitrarily inorganic material that is suitable for that all the other compositions of described inorganic nano-filler can allow; The preferred material of all the other compositions of described inorganic nano-filler is a kind of of following material at least: nanometer hydroxyapatite, biological glass powder, commercially available barium lead glass powder, strontium glass powder, boron lead glass powder, barium strontium boron glass powder, certainly, also can be the combination of two or more listed alternative materials.
This case dental resin composition also is a kind of dentistry compound resin material certainly.
The related flaky silicon dioxide granule of this case, its technology of preparing and manufactured goods, Merck KGaA company can provide, and city's spot sale is arranged on the Chinese domestic market; In addition, the particulate preparation method of flaky silicon dioxide also can be sought from the Chinese and English scientific and technical literature.
Related other related reagent of this case and material all have finished product commercially available; The corresponding technology of preparing that related other related reagent and material also can utilize relevant speciality Gao Ke company to provide with compensation prepares to be obtained; Certainly, related other related reagent and material can also be obtained by the mode to relevant speciality Gao Ke company customization finished product.
This case dental resin composition can also comprise some other compositions certainly, the for example an amount of polymerization inhibitor of described other composition, an amount of polymerization inhibitor can be kept the effective life of dental resin composition, and described polymerization inhibitor can be selected aldehydes matter for use, and the polymerization inhibitor composition is optional; The coloring agent that described other composition is also for example an amount of, an amount of coloring agent can be given dental resin composition after the curing with the natural teeth color and luster, are suitable for optional coloring agent such as the titanium white of this purpose and chrome yellow etc., and described coloring agent component is optional.
Advantage of the present invention is, described photocuring dental resin composition contains the flaky silicon dioxide particulate component, to be that this case is critical be used to increase anti-wear performance to the flaky silicon dioxide particulate component, increase the material composition of toughness and tenacity, the flaky silicon dioxide granule has the inherent moderate hardness of silicon dioxide, and, in the composite resin oberbau after in application, solidifying, the particulate lamellar pattern of flaky silicon dioxide, also make the flaky silicon dioxide granule be positioned on the surface layer to have more multimachine can wedge the composite resin matrix dearly than circular granular or amorphous granular, in other words, more strong comparatively speaking at flaky silicon dioxide granule on the surface layer and the adhesion between the composite resin matrix, this factor, make the flaky silicon dioxide granule that is positioned on the surface layer among using, be difficult for being peeled off by friction strength, therefore the flaky silicon dioxide granule that is positioned on the surface layer can be anchored on the composite resin more muchly, bringing into play the front to increasing wearability that its high rigidity brings more muchly benefits, that is to say that this helps to reduce the abrasion speed of composite resin; On the other hand, composite resin matrix inside after the photocuring in application, disperse a large amount of flaky silicon dioxide granule therebetween changes bending, distortion and fracture more intense drag, this stems to a great extent extracts toughening effect, and this factor helps to improve the toughness of composite resin; And; have the plate granule-morphology that the flaky silicon dioxide granule is also laminar because of it and size is small that benefit in front, above-mentioned two aspect, comparatively speaking, in preparation process than other composition uniform mixing that is easier to this case compositions; in other words, be not prone to the mixing obstacle in the preparation process.
The specific embodiment
Embodiment 1:
Take by weighing 10.00 gram flaky silicon dioxide granules, and, 50.00 gram barium strontium boron glass powder, and 40.00 gram boron lead glass powder carry out uniform mixing by churned mechanically mode with above three kinds of compositions, make gross weight and be the nano inorganic powder that contains multiple composition of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 2.50 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 40 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 70 to 30, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains multiple composition of 22.00 grams, in ultrasound wave, disperse, afterwards, reaction is 24 hours under 50 ℃ of temperature, moves to baking oven, dries 10 hours down at 80 ℃, then, with described water-alcohol solution washing, dried 10 hours down in 100 ℃ again, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
In 70.00 gram bisphenol-A glycidyl methacrylate, add 5.00 gram double methyl methacrylate triethylene glycol ester dilutions, stir, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 2.00 gram camphorquinones and 3.00 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 20.00 the gram these routine described modifications after nano inorganic powder, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 10 minutes places vacuum desiccator with mixture, application of vacuum 24 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 2:
Take by weighing 80.00 gram flaky silicon dioxide granules, and, 15.00 gram barium strontium boron glass powder, and 5.00 gram nanometer hydroxyapatites carry out uniform mixing by churned mechanically mode with above three kinds of compositions, make gross weight and be the nano inorganic powder that contains multiple composition of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 2.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 400 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 5 to 95, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains multiple composition of 87.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 2 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 8.00 gram bisphenol-A glycidyl methacrylate, add 6.25 gram double methyl methacrylate triethylene glycol ester dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 0.25 gram camphorquinone and 0.50 gram dimethylaminoethyl acrylate methyl ammonia ethyl ester are mixed, after mixing, add therein 85.00 the gram these routine described modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 2 hours, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 10 hours, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 3:
Take by weighing 45.00 gram flaky silicon dioxide granules, and, 25.00 gram barium strontium boron glass powder, and, 10.00 gram nanometer hydroxyapatites, and, 5.00 gram strontium glass powder, and, 5.00 gram boron lead glass powder, and, 10.00 restrain commercially available barium lead glass powder, by churned mechanically mode above multiple composition is carried out uniform mixing, make gross weight and be the nano inorganic powder that contains multiple composition of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 10.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 200 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 2.4 to 1.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains multiple composition of 55.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 39.00 gram bisphenol-A glycidyl methacrylate, add 5.59 gram double methyl methacrylate triethylene glycol ester dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.16 gram camphorquinones and 1.75 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 52.50 the gram these routine described modifications after the nano inorganic powder that contains multiple composition, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 45 minutes, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 16 hours, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 4:
Take by weighing 30.00 gram flaky silicon dioxide granules, and, 30.00 gram barium strontium boron glass powder, and, 10.00 gram biological glass powders, and, 5.00 gram strontium glass powder, and, 5.00 gram boron lead glass powder, and, 20.00 restrain commercially available barium lead glass powder, by churned mechanically mode above multiple composition is carried out uniform mixing, make gross weight and be the nano inorganic powder that contains multiple composition of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 5.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 200 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains multiple composition of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 40.00 gram bisphenol-A glycidyl methacrylate, add 25.00 gram double methyl methacrylate triethylene glycol ester dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram these routine described modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 20 hours, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 5:
Take by weighing 60.00 gram flaky silicon dioxide granules, and the commercially available barium lead glass powder of 40.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, and is standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 50.00 gram carbamate double methyl methacrylates, add 15.00 gram Ethylene glycol dimethacrylate dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram these routine described modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 20 hours, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 6:
Take by weighing 70.00 gram flaky silicon dioxide granules, and the strontium glass powder of 30.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 20.00 gram carbamate double methyl methacrylates, and get 30.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 15.00 gram hydroxyethyl methylacrylate dilutions, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add the nano inorganic powder that contains multiple composition after these routine described modifications of 32.80 grams therein, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 7:
Take by weighing 75.00 gram flaky silicon dioxide granules, and the commercially available barium lead glass powder of 25.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 20.00 gram carbamate double methyl methacrylates, and get 20.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 10.00 gram double methyl methacrylate triethylene glycol esters, 10.00 gram Ethylene glycol dimethacrylate, 5.00 gram hydroxyethyl methylacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram these routine described modifications after the nano inorganic powder that contains multiple composition, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 8:
Take by weighing 65.00 gram flaky silicon dioxide granules, and the commercially available boron lead glass powder of 35.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 10.00 gram carbamate double methyl methacrylates, and get 30.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 15.00 gram double methyl methacrylate triethylene glycol esters, 10.00 gram Ethylene glycol dimethacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram these routine described modifications after the nano inorganic powder that contains multiple composition, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 9:
Take by weighing 10.00 gram flaky silicon dioxide granules, and the commercially available biological glass powder of 90.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 4.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 6.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 75 ℃ of temperature, reacted 15 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 30.00 gram carbamate double methyl methacrylates, and get 10.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 10.00 gram double methyl methacrylate triethylene glycol esters, 15.00 gram Ethylene glycol dimethacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram these routine described modifications after the nano inorganic powder that contains multiple composition, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 10:
Take by weighing 40.00 gram flaky silicon dioxide granules, and, the biological glass powder of 30.00 grams, 30.00 the nanometer hydroxyapatite of gram, by churned mechanically mode above two kinds of compositions are carried out uniform mixing, make gross weight and be the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and, the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40, and all flaky silicon dioxide granular materialss that satisfies the limited proportion of described plate width qualification and described plate width and sheet all can use.
With 5.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 5.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 60 ℃ of temperature, reacted 20 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement.
Get 30.00 gram carbamate double methyl methacrylates, and get 20.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 10.00 gram double methyl methacrylate triethylene glycol esters, 5.00 gram Ethylene glycol dimethacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram these routine described modifications after the nano inorganic powder that contains multiple composition, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Claims (10)
1. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 10.00 gram flaky silicon dioxide granules, and, 50.00 gram barium strontium boron glass powder, and 40.00 gram boron lead glass powder carry out uniform mixing by churned mechanically mode with above three kinds of compositions, make gross weight and be the nano inorganic powder of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 2.50 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 40 ml water alcoholic solutions, water, pure volume ratio are 70 to 30 in this water-alcohol solution, subsequently, the above-mentioned mixed in advance nano inorganic powder that adds 22.00 grams, disperse in ultrasound wave, afterwards, reaction is 24 hours under 50 ℃ of temperature, move to baking oven, dried 10 hours down at 80 ℃, then, with described water-alcohol solution washing, dried 10 hours down in 100 ℃ again, after the drying, pulverize, make the nano inorganic powder after the modification;
In 70.00 gram bisphenol-A glycidyl methacrylate, add 5.00 gram double methyl methacrylate triethylene glycol ester dilutions, stir, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 2.00 gram camphorquinones and 3.00 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 20.00 the gram modifications after nano inorganic powder, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 10 minutes places vacuum desiccator with mixture, application of vacuum 24 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth.
2. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 80.00 gram flaky silicon dioxide granules, and, 15.00 gram barium strontium boron glass powder, and 5.00 gram nanometer hydroxyapatites carry out uniform mixing by churned mechanically mode with above three kinds of compositions, make gross weight and be the nano inorganic powder of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 2.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 400 ml water alcoholic solutions, water, pure volume ratio are 5 to 95 in this water-alcohol solution, subsequently, add the above-mentioned mixed in advance nano inorganic powder of 87.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 2 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 8.00 gram bisphenol-A glycidyl methacrylate, add 6.25 gram double methyl methacrylate triethylene glycol ester dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 0.25 gram camphorquinone and 0.50 gram dimethylaminoethyl acrylate methyl ammonia ethyl ester are mixed, after mixing, add therein 85.00 the gram modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 2 hours, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 10 hours, make photo-curing composition for tooth.
3. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 45.00 gram flaky silicon dioxide granules, and, 25.00 gram barium strontium boron glass powder, and, 10.00 gram nanometer hydroxyapatites, and, 5.00 gram strontium glass powder, and, 5.00 gram boron lead glass powder, and, 10.00 restrain commercially available barium lead glass powder, by churned mechanically mode above multiple composition is carried out uniform mixing, make gross weight and be the nano inorganic powder of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 10.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 200 ml water alcoholic solutions, water, pure volume ratio are 2.4 to 1.0 in this water-alcohol solution, subsequently, add the above-mentioned mixed in advance nano inorganic powder of 55.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 39.00 gram bisphenol-A glycidyl methacrylate, add 5.59 gram double methyl methacrylate triethylene glycol ester dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.16 gram camphorquinones and 1.75 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 52.50 the gram modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 45 minutes, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 16 hours, make photo-curing composition for tooth.
4. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 30.00 gram flaky silicon dioxide granules, and, 30.00 gram barium strontium boron glass powder, and, 10.00 gram biological glass powders, and, 5.00 gram strontium glass powder, and, 5.00 gram boron lead glass powder, and, 20.00 restrain commercially available barium lead glass powder, by churned mechanically mode above multiple composition is carried out uniform mixing, make gross weight and be the nano inorganic powder of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 5.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 200 ml water alcoholic solutions, water, pure volume ratio are 1.0 to 10.0 in this water-alcohol solution, subsequently, add the above-mentioned mixed in advance nano inorganic powder of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 40.00 gram bisphenol-A glycidyl methacrylate, add 25.00 gram double methyl methacrylate triethylene glycol ester dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 20 hours, make photo-curing composition for tooth.
5. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 60.00 gram flaky silicon dioxide granules, and the commercially available barium lead glass powder of 40.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, and is standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, again in 80 ℃ of down oven dry 12 hours, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby, reserve level is slightly greater than requirement;
Get 50.00 gram carbamate double methyl methacrylates, add 15.00 gram Ethylene glycol dimethacrylate dilutions therein, both are stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram modifications after nano inorganic powder, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes, mixture is placed vacuum desiccator, the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 20 hours, make photo-curing composition for tooth.
6. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 70.00 gram flaky silicon dioxide granules, and the strontium glass powder of 30.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 20.00 gram carbamate double methyl methacrylates, and get 30.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 15.00 gram hydroxyethyl methylacrylate dilutions, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add the nano inorganic powder after the modifications of 32.80 grams therein, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth.
7. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 75.00 gram flaky silicon dioxide granules, and the commercially available barium lead glass powder of 25.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 20.00 gram carbamate double methyl methacrylates, and get 20.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 10.00 gram double methyl methacrylate triethylene glycol esters, 10.00 gram Ethylene glycol dimethacrylate, 5.00 gram hydroxyethyl methylacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram modifications after nano inorganic powder, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth.
8. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 65.00 gram flaky silicon dioxide granules, and the commercially available boron lead glass powder of 35.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 10.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 100 ℃ of temperature, reacted 2 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 10.00 gram carbamate double methyl methacrylates, and get 30.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 15.00 gram double methyl methacrylate triethylene glycol esters, 10.00 gram Ethylene glycol dimethacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram modifications after nano inorganic powder, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth.
9. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 10.00 gram flaky silicon dioxide granules, and the commercially available biological glass powder of 90.00 grams carries out uniform mixing by churned mechanically mode with above two kinds of compositions, makes gross weight and is the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 4.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 6.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 75 ℃ of temperature, reacted 15 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 30.00 gram carbamate double methyl methacrylates, and get 10.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 10.00 gram double methyl methacrylate triethylene glycol esters, 15.00 gram Ethylene glycol dimethacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add therein 32.80 the gram modifications after nano inorganic powder, carrying out mechanical agitation mixes, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth.
10. photo-curing composition for tooth, it prepares with the following method:
Take by weighing 40.00 gram flaky silicon dioxide granules, and, the biological glass powder of 30.00 grams, 30.00 the nanometer hydroxyapatite of gram, by churned mechanically mode above two kinds of compositions are carried out uniform mixing, make gross weight and be the nano inorganic powder that contains two kinds of compositions of 100.00 grams, standby; The particulate plate width of wherein related flaky silicon dioxide is between 0.3 micron and 36.0 microns, and the ratio of particulate plate width of related flaky silicon dioxide and sheet is between 3 and 40;
With 5.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water in this water-alcohol solution, the alcohol volume ratio is 1.0 to 5.0, subsequently, add the above-mentioned mixed in advance nano inorganic powder that contains two kinds of compositions of 35.00 grams, in ultrasound wave, disperse, under 60 ℃ of temperature, reacted 20 hours afterwards, move to baking oven, dried 2 hours down at 80 ℃ earlier, then, with described water-alcohol solution washing, dried 12 hours down in 80 ℃ again, after be warming up to 100 ℃ and continue oven dry 5 hours, after the drying, pulverize, make the nano inorganic powder after the modification, standby;
Get 30.00 gram carbamate double methyl methacrylates, and get 20.00 gram bisphenol-A glycidyl methacrylate, in the above two mixture, add 10.00 gram double methyl methacrylate triethylene glycol esters, 5.00 gram Ethylene glycol dimethacrylate dilution, this mixture system is stirred, make resinous substrates, thereafter, under the lucifuge condition, the resinous substrates made and 1.00 gram camphorquinones and 1.20 gram dimethylaminoethyl acrylate methyl ammonia ethyl esters are mixed, after mixing, add the nano inorganic powder after the modifications of 32.80 grams therein, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 20 minutes places vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make photo-curing composition for tooth.
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| CN102060702B (en) * | 2010-10-28 | 2013-12-25 | 华南理工大学 | Visible light curing fluorine-containing dental resin monomer/composite material and preparation method thereof |
| CN102973416B (en) * | 2012-12-07 | 2014-07-23 | 东华大学 | Preparation method of dental restoring resin taking silicon dioxide and cluster of silicon dioxide as stuffing |
| CN103356391B (en) * | 2013-04-17 | 2015-04-29 | 安泰科技股份有限公司 | Dual curing crown nuclear resin for dentistry and preparation method thereof |
| CN104940026A (en) * | 2015-06-01 | 2015-09-30 | 张亚南 | Dental material for dental caries repair and preparation method thereof |
| CN106539694A (en) * | 2016-12-09 | 2017-03-29 | 苏州纳贝通环境科技有限公司 | A kind of hard tooth tissue adhesive and preparation method thereof |
| CN106821768B (en) * | 2017-01-22 | 2020-06-16 | 广西纳维天使医疗器械有限公司 | Photo-curing biological anti-caries tooth repair material and preparation method thereof |
| CN107245314A (en) * | 2017-05-26 | 2017-10-13 | 苏州汉力新材料有限公司 | A kind of 3D printing powder ultraviolet light curing adhesive and preparation method thereof |
| CN109714686B (en) * | 2018-12-24 | 2020-07-17 | 湖北冠音泰科技有限公司 | Super linear loudspeaker |
| CN110092652A (en) * | 2019-04-23 | 2019-08-06 | 四川大学 | Bioactivity, porous ceramic preparation based on the face DLP exposure forming technique |
| CN110724406B (en) * | 2019-11-27 | 2022-09-20 | 九牧厨卫股份有限公司 | Modified flaky silicon dioxide, scratch-resistant easy-to-clean hand feeling coating and preparation method thereof |
| CN114522107A (en) * | 2020-11-23 | 2022-05-24 | 松山湖材料实验室 | Dental adhesive and method for preparing dental product |
| CN113499269A (en) * | 2021-06-05 | 2021-10-15 | 北京化工大学 | Dental restoration composite resin with dual functions of bacteriostasis and remineralization as well as preparation and application thereof |
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| GB1428165A (en) * | 1972-03-21 | 1976-03-17 | Dentsply Int Inc | Compositions for use in dentistry |
| CN1951358A (en) * | 2006-11-09 | 2007-04-25 | 深圳清华大学研究院 | A method for preparing nano compound resin prosthetics material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1428165A (en) * | 1972-03-21 | 1976-03-17 | Dentsply Int Inc | Compositions for use in dentistry |
| CN1951358A (en) * | 2006-11-09 | 2007-04-25 | 深圳清华大学研究院 | A method for preparing nano compound resin prosthetics material |
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