CN101669882B - Preparation method of dental material based on photochemical fast reaction mechanism - Google Patents
Preparation method of dental material based on photochemical fast reaction mechanism Download PDFInfo
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Abstract
The invention relates to a preparation method of a dental material based on a photochemical fast reaction mechanism, which relates to the field of dental preparation. The scheme aims at solving the problem that the existing dental material used for filling caries needs to be further improved in the aspects of abrasion resistance and toughness. The method comprises the steps of utilizing silane coupling agent to conduct surface modification to inorganic nano-powder; evenly mixing the modified inorganic nano-powder with bisphenol A glycidyl methacrylate monomer, triethylene-glycol dimethacrylate thinner, camphorquinone photo-initiator and dimethylamino ethyl methacrylate coinitiator and the like under a condition without sunlight; and removing bubbles under a vacuum condition. The key point of the scheme is as follows: the inorganic nano-powder contains alumina nano-tube which accounts for 10 to 80 percent of weight of the inorganic nano-powder. The alumina nano-tube added in the inorganic nano-powder is beneficial to improving the anchoring force and increasing the toughness due to the feature and toughness thereof.
Description
Technical field
The present invention relates to a kind of preparation method of dental material, belong to that A61K is medical, the dental preparation field based on photochemical fast reaction mechanism.
Background technology
Repair in all kinds of dental materials of usefulness in the nest hole, compare based on the single paste type light-cured composite of photochemical fast reaction mechanism and to have tangible comprehensive advantage, just owing to this reason, generally accepted this emerging composite in the nest hole repair of tooth section, though so, such material is further improved with perfect still very necessary.
In tooth section nest hole is repaired with each composition of dentistry composite resin, for amorphous granular is adopted in the inorganic filler of gaining in strength and wearability adds more, its particle outline of amorphous granular is similar to sphere roughly, the effect that it can be brought into play in tooth section nest hole is repaired with composite resin also is similar to spheroidal particle, repair the surface layer of using dentistry composite resin in the tooth section nest hole 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, the effect that this factor makes amorphous granular repair aspect the dentistry composite resin wearability in lifting tooth section nest hole is made a discount, on the other hand, repair with in the dentistry composite resin body in tooth section nest hole after solidifying, the rough approximation substantially of amorphous granular is in spheric pattern, repairs to contribute also because of fully not taking into account with the Strengthening and Toughening of dentistry composite resin for tooth section nest hole and extracts toughening mechanisms some shortcomings have been arranged.
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 dentistry composite resin anti-wear performance and toughness and tenacity, develop a kind of new preparation method for dental fortified resin, this method should be taken the raising of wearability into account, also will take into account to extract toughening mechanisms the front of Strengthening and Toughening is benefited.
The present invention solve the technical problem by following scheme, this scheme provides a kind of preparation method of dental material based on photochemical fast reaction mechanism, and this method may further comprise the steps: (1) forms silane coupler hydrolysis under acetic acid catalysis the water alcohol system that contains coupling agent; (2) nano inorganic powder is added ultra-sonic dispersion in the water alcohol system that contains coupling agent, after reacting completely, washing, drying obtain the inorganic nano-filler of modification; (3) resin monomer is added an amount of diluent dilution, form resinous substrates with good miscibility; (4) under the lucifuge condition, the resinous substrates for preparing is added light trigger and coinitiator, after stirring, add the inorganic nano-filler of modification again, behind the mix homogeneously, remove interlaminar resin and have bubble, prepare nano-composite resin material; It is characterized in that it is 10%～80% alumina nano tube that described nano inorganic powder contains the percetage by weight that accounts for nano inorganic powder weight; The external diameter of described alumina nano tube is between 3 nanometers and 10 nanometers, and the length of described alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of described alumina nano tube and external diameter is between 3 and 70.The alumina nano tube that radial width and longitudinal length all belong to the nanosecond science and technology size category not only helps reducing the operation easier of raw material mixed processes, and, obviously, it also helps the stability that increases the finished product paste, simultaneously, increase the flowability of finished product paste, and the raising of the mobile performance of finished product paste, then help to reduce the operation easier of this finished product paste clinical practice.
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, the operation that an amount of diluent of adding dilutes in step (3) is necessary, the adding 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.
This case dentistry compound resin material is described dental material based on photochemical fast reaction mechanism, and this material 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, for example, situation to the KH-570 that selects medical grade for use, when disposing described water alcohol system, wherein the scope that water and the volume ratio of alcohol are optionally suitable is 5 to 95～70 to 30.
Utilize silane coupler nano inorganic powder to be carried out the result of modification, just coat the coupling agent molecule layer of about one deck molecular layers thick of skim on the surface of nano inorganic powder, thereby, the actual coupling agent requirement that plays a role is also few, in described water alcohol system, the suitable weight percentage of silane coupler is 0.5%～10%, and, in step (2), nano inorganic powder is 1 to 20～1 to 2 with the suitable weight ratio scope of water alcohol system.
In the described step of this case (2), the reaction temperature preferable range is 50 ℃～100 ℃, and the response time, preferred yardstick was between 2h～24h.Certainly, reaction temperature and response time also can allow to do as required other selection.
Not allowing bubble in the finished product dentistry composite resin is mingled with therebetween, in addition, unnecessary tool is volatile to be mingled with the complementary composition that other permission therebetween is added into and also must to remove in operating process, there is kind of mode can reach this purpose, in the described step of this case (4), preferably remove the mode of bubble and other volatile impurity, be by ultrasonication 10min～2h then the mode of vacuum drying effect 10h～24h remove the bubble that exists in the resin.
In the described step of this case (4), the weight percentage apportioning cost of each component can be the rational arbitrarily apportioning cost of setting as required in the nanocomposite, but, based on the demand of the described dentistry composite resin of this case at aspect of performance, the preferable range of the weight percentage of each component is respectively in the described nanocomposite: the inorganic nano-filler 20%～85% after resin monomer 8%～70%, diluent 5%～25%, light trigger 0.25%～2%, coinitiator 0.5%～3%, the modification.
Above address, it is 1%～80% alumina nano tube 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.
The technology of preparing of the related alumina nano tube of this case can be sought from existing scientific and technical literature, relevant scientific and technical literature is for example: the application for a patent for invention case that is entitled as " a kind of alumina nano tube and its production and application " that Dalian Inst of Chemicophysics, Chinese Academy of Sciences submitted to JIUYUE in 2005 on the 8th, open day of this case is on March 14th, 2007, the publication number of this case is CN 1927696A, and the application number of this application case is 200510086373.6.
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.
In described step (1), step (3), can add ultrasound wave effect operation, utilize ultrasound wave to be used for promoting reaction or acceleration uniform mixing, certainly, the operation that can add the ultrasound wave effect in described step (1), step (3) is optional; Mix stages in step (4) can further add ultrasound wave effect operation, and this helps to facilitate the uniform mixing of each composition, but that ultrasound wave acts on this link is optional, because the conventional mode that mixes is also effective.
This case method can also comprise some other steps certainly, described other step for example adds an amount of polymerization inhibitor in described nano-composite resin material system, add an amount of polymerization inhibitor and its objective is the effective life of keeping nanocomposite, described polymerization inhibitor can be selected aldehydes matter for use, and the step that adds polymerization inhibitor is optional; Described other step also for example adds an amount of coloring agent in described nano-composite resin material system, adding an amount of coloring agent its objective is and give resin with the natural teeth color and luster, be suitable for optional coloring agent such as the titanium white of this purpose and chrome yellow etc., described coloring agent also can add wherein.
Advantage of the present invention is, this method utilizes the alumina nano tube composition as critical increase wearability, increase flexible material composition, alumina nano tube has high rigidity, and, in resin surface layer is constructed after solidifying in application, the tubulose pattern of alumina nano tube, make that also being positioned at alumina nano tube on the surface layer can have more that multimachine can be rooted in resin matrix dearly than circular granular or amorphous granular, in other words, adhesion between alumina nano tube on the surface layer and composite resin matrix is more strong comparatively speaking, this factor, make the alumina nano tube that is positioned on the surface layer among using, be difficult for being peeled off by friction strength, therefore the alumina nano tube that is positioned on the surface layer can be anchored on the surface of 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 in application, solidifying, disperse a large amount of alumina nano tube therebetween changes bending, distortion and fracture more intense drag, and this stems to a great extent extracts toughening effect, and this factor helps to improve the toughness of composite resin.
The effect of alumina nano tube in described dentistry compound resin material is similar to the steel-pipe pile that adopts in the civil construction project in a measure, communicates on the principle.
The specific embodiment
Embodiment 1:
Take by weighing 10.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 2:
Take by weighing 80.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, and making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 3:
Take by weighing 45.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, and making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 4:
Take by weighing 30.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, and making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 5:
Take by weighing 60.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, and making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 6:
Take by weighing 70.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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 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, making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 7:
Take by weighing 75.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 8:
Take by weighing 65.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 9:
Take by weighing 10.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Embodiment 10:
Take by weighing 40.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and, the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and, the ratio of the length of related alumina nano tube and external diameter is between 3 and 70, and all aluminium oxide nano tube materials that satisfies described qualification 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, making nano-composite resin material is the described dental material based on photochemical fast reaction mechanism of this case; Can under lucifuge condition according to usual use amount carry out finished product packing thereafter.
Claims (10)
1. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 10.00 gram alumina nano tubes, 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 are the nano inorganic powder of 100.00 grams, and are standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
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, add the above-mentioned mixed in advance nano inorganic powder of 22.00 grams, in ultrasound wave, disperse, 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, standby;
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 was finished, ultrasound wave effect 10 minutes placed vacuum desiccator with mixture, application of vacuum 24 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
2. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 80.00 gram alumina nano tubes, 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 are the nano inorganic powder of 100.00 grams, and are standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
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 the nano inorganic powder after the modifications of 85.00 grams therein, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 2 hours, mixture is placed vacuum desiccator, and the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 10 hours, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
3. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 45.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
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 the nano inorganic powder after the modifications of 52.50 grams therein, carry out mechanical agitation and mix, after the mechanical agitation married operation is finished, ultrasound wave effect 45 minutes, mixture is placed vacuum desiccator, and the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 16 hours, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
4. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 30.00 gram alumina nano tubes, 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; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
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 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, mixture is placed vacuum desiccator, and the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 20 hours, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
5. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 60.00 gram alumina nano tubes, 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 of 100.00 grams, and is standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 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 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 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, mixture is placed vacuum desiccator, and the bubble and other volatile impurity that are mingled with in the mixture are removed in application of vacuum 20 hours, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
6. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 70.00 gram alumina nano tubes, 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 of 100.00 grams, standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 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 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, carrying out mechanical agitation mixes, after the mechanical agitation married operation was finished, ultrasound wave effect 20 minutes placed vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
7. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 75.00 gram alumina nano tubes, 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 of 100.00 grams, standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 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 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 was finished, ultrasound wave effect 20 minutes placed vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
8. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 65.00 gram alumina nano tubes, 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 of 100.00 grams, standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
With 3.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 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 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 was finished, ultrasound wave effect 20 minutes placed vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
9. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 10.00 gram alumina nano tubes, 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 of 100.00 grams, standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
With 4.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water, pure volume ratio are 1.0 to 6.0 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 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 was finished, ultrasound wave effect 20 minutes placed vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
10. preparation method of dental material based on photochemical fast reaction mechanism, form by following steps:
Take by weighing 40.00 gram alumina nano tubes, and, the biological glass powder of 30.00 grams, the nanometer hydroxyapatite 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 of 100.00 grams, and is standby; Wherein the external diameter of related alumina nano tube is between 3 nanometers and 10 nanometers, and the length of related alumina nano tube is between 10 nanometers and 200 nanometers, and the ratio of the length of related alumina nano tube and external diameter is between 3 and 70;
With 5.00 gram medical grade silane coupler KH-570 hydrolysis under the effect of acetic acid, add 100 ml water alcoholic solutions, water, pure volume ratio are 1.0 to 5.0 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 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 therein 32.80 the gram modifications after nano inorganic powder, carrying out mechanical agitation mixes, after the mechanical agitation married operation was finished, ultrasound wave effect 20 minutes placed vacuum desiccator with mixture, application of vacuum 20 hours, remove the bubble and other volatile impurity that are mingled with in the mixture, make nano-composite resin material, promptly based on the dental material of photochemical fast reaction mechanism.
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