CN103284888A - Calcium hydroxide hydrophilic resin - Google Patents
Calcium hydroxide hydrophilic resin Download PDFInfo
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- CN103284888A CN103284888A CN2013102428160A CN201310242816A CN103284888A CN 103284888 A CN103284888 A CN 103284888A CN 2013102428160 A CN2013102428160 A CN 2013102428160A CN 201310242816 A CN201310242816 A CN 201310242816A CN 103284888 A CN103284888 A CN 103284888A
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- collagen
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- calcium hydroxide
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- mineralising
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Abstract
The invention provides a calcium hydroxide hydrophilic resin. The calcium hydroxide hydrophilic resin is prepared from hydrophilic resin matrix, inorganic filler and a collagen mineralization inducer, wherein the hydrophilic resin matrix is prepared from camphorquinone, 4-(N, N-dimethyl amine) ethyl benzoate, ethoxyl methyl methacrylate and bisphenol A dimethyl glycidyl acrylate; the inorganic filler is silanized gas-phase nanometer silicon dioxide; the collagen mineralization inducer is calcium hydroxide; the improvement is that the ratio (in parts by weight) of the hydrophilic resin matrix to the inorganic filler to the collagen mineralization inducer is 4:1:5; the collagen mineralization inducer is nanometer calcium hydroxide. The alkaline environment is kept by providing dilution of hydroxyl ions, so that the collagen fiber is induced to re-mineralize, and therefore, the dentin is promoted to re-mineralize; the calcium ion concentration around the tooth tissue can be kept by virtue of the calcium ion dilution, so that a calcium ion source is provided for re-mineralization of collagen and dentin re-mineralization to realize the dentin mineralization, and therefore, the calcium hydroxide hydrophilic resin is an ideal clinical dental material.
Description
Technical field
The present invention relates to dental materials, relate in particular to a kind of calcium hydroxide hydrophilic resin with dentin remineralization inducibility.
Background technology
Dentinal remineralization and collagen fiber are closely related, and mineral is divided in the fiber mineralising between mineralising and fiber in the dentin collagen mineralising, and the former refers to form orderly apatite precipitation in porose area in collagen fiber and the hole; The latter refers to that the apatite precipitation occupies the space that separates between the collagen fiber.Experiment in vitro is verified: the mineralising in the collagen fiber is by complicated reacting to each other and orderly formation between collagen stroma and the noncollagen protein.But still mineralising between fiber in the fiber no matter, alkaline environment is the essential condition of collagen mineralising.At present, the material that can be applicable to remineralization has poly-acid modified resin, and it is fixed against fluoride and carries out remineralization, is primarily aimed at enamel, does not meet Dentinal remineralization mechanism; Calcium hydroxide paste, usually by as the direct pulp capping agent, the examination that is applied to dark dental caries is mended, and is not final obturator; Three oxidation mineralising polymers (MTA), it has better biocompatibility and calcium ion slow-releasing system, but (MTA) need hydration to make its curing, the repeatedly further consultation of clinical common needs, scholar's handle (MTA) is arranged after external being cured, make (MTA) hydrophilic resin with mixed with resin, this resin both had the calcium hydroxide active component after (MTA) curing, also can be used as final obturator, thereby reduced patient's number of times of going to a doctor, be a kind of dentin remineralization resin material commonly used in the present scientific research, fail to understand but (MTA) solidify the effect of other compositions of back in mineralising.
Pass through correlational study, dentin remineralization material require hydroxyl and calcium ion slow-releasing system are induced collagen and Dentinal remineralization, simultaneously should be as final obturator, therefore mix with resinous substrates by the former mineralising derivant of direct rubber polymer and by proper proportion, make material property that further improvement be arranged, present clinical oral cavity material is needed badly.
Summary of the invention
Main purpose of the present invention is to overcome the above-mentioned shortcoming that existing product exists, and a kind of oxygen calcium oxide hydrophilic resin is provided, and it can provide the slow release of hydroxide ion to keep alkaline environment, thereby induces the collagen fiber remineralization, promotes the dentin remineralization; The slow release of its calcium ion can be kept calcium ion concentration around the tissue of tooth, for collagen and dentin remineralization provide the calcium ion source, thereby realizes the dentin mineralising, is desirable clinical oral cavity material.
The objective of the invention is to be realized by following technical scheme.
Calcium hydroxide hydrophilic resin of the present invention, formed by hydrophilic resin substrate, inorganic filler and the configuration of collagen mineralising derivant, this hydrophilic resin substrate is formed by camphorquinone, 4-(N, N-diformazan ammonia) ethyl benzoate, ethoxy methyl methacrylate and the configuration of bisphenol-A methacrylate ethylene oxidic ester; This inorganic filler is the gas phase nano silicon dioxide of silanization; It is characterized in that the ratio of weight and number of described hydrophilic resin substrate, inorganic filler and collagen mineralising derivant is: hydrophilic resin substrate: inorganic filler: collagen mineralising derivant=4: 1: 5; Described collagen mineralising derivant is the nanoscale calcium hydroxide.
The beneficial effect of calcium hydroxide hydrophilic resin of the present invention, it can provide the slow release of hydroxide ion to keep alkaline environment, thereby induces the collagen fiber remineralization, promotes the dentin remineralization; The slow release of its calcium ion can be kept calcium ion concentration around the tissue of tooth, for collagen and dentin remineralization provide the calcium ion source, thereby realizes the dentin mineralising, is desirable clinical oral cavity material.In addition, this resin and (MTA) resin comparison, its hydrophilic is better than (MTA) resin, nanoscale calcium hydroxide in this resin can improve the hydrophilic of dental filling material, and certain biocidal property arranged, the cost of dentin remineralization material is reduced, and therefore this material is applied in the clinical dental care satisfactory for result.
The specific embodiment
Calcium hydroxide hydrophilic resin of the present invention, formed by hydrophilic resin substrate, inorganic filler and the configuration of collagen mineralising derivant, this hydrophilic resin substrate is formed by camphorquinone, 4-(N, N-diformazan ammonia) ethyl benzoate, ethoxy methyl methacrylate and the configuration of bisphenol-A methacrylate ethylene oxidic ester; This inorganic filler is the gas phase nano silicon dioxide of silanization; Its improvements are that the ratio of weight and number of described hydrophilic resin substrate, inorganic filler and collagen mineralising derivant is: hydrophilic resin substrate: inorganic filler: collagen mineralising derivant=4: 1: 5; Described collagen mineralising derivant is the nanoscale calcium hydroxide.
Embodiment 1:
(1) configuration hydrophilic resin substrate: take by weighing 25 gram camphorquinones, 1 gram 4-(N, N-diformazan ammonia) ethyl benzoate, 38.75 gram ethoxy methyl methacrylates and 60 gram bisphenol-A methacrylate ethylene oxidic esters, under lucifuge and normal temperature and pressure conditions, standby after the mixing and stirring;
(2) preparation inorganic filler: get the 20mL dehydrated alcohol, add 2mL silane coupler and 2mL acetic acid solution and mix, 0.5g gas phase nano silicon dioxide is added in the solution stir ultrasonic concussion 30 minutes, 55 ℃ of waters bath with thermostatic control 5 hours, see white clear gel, centrifugalize, solid cleans 3 times with dehydrated alcohol, dry 24 hours, obtain the nano-silica powder end of silanization, powder is flooded with mortar, all preserve by sealing behind 400 eye mesh screens.
(3) the former mineralising derivant of rubber polymer action component: the 0.98g polyvinyl alcohol is poured in the 50mmL deionized water continuously, slowly be heated to 100 ℃, and stirred accelerate dissolution 1 hour.With solution left standstill 2 hours, treat lather collapse after the dissolving, standardize solution 100mL makes the clarification poly-vinyl alcohol solution.Get 25ml 0.17M calcium chloride solution, the 6mL poly-vinyl alcohol solution places dry sealed reagent bottle, ultrasonic concussion 1 hour, ageing 12 hours.Add magneton subsequently, use peristaltic pump that the 50mL0.17M sodium hydroxide solution is injected reagent bottle, reagent bottle places magnetic stirring apparatus to stir, and the control rotating speed is 1 revolutions per second, and a speed of peristaltic pump is 10mL/ hour.React after 1 hour the visible solution turbid solution that is white in color.After the sodium hydroxide titration is finished, the ultrasonic concussion of reactant was seen the white particle precipitation in the bottle end after 30 minutes, solution centrifugal 30 minutes, 4000 rev/mins, remove supernatant, precipitate uses absolute ethanol washing three times, filters, centrifugalize, condition is the same.To precipitate natural drying 24 hours, namely make the nano calcium hydroxide powder.Show under this calcium hydroxide transmission electron microscope: granule presents homodisperse nanosphere, and the granule mean diameter is less than 100nm, the complete rule of form rule.
(4) get the silicon dioxide (SiO of hydrophilic hybrid resin 40mg, silanization
2) powder 10mg, nano calcium hydroxide powder 50mg lucifuge transfer and mix evenly, remove bubble, inject the Teflon mould, for preventing that airborne oxygen from influencing resin polymerization, transparent Mylar polyester strip is covered the resin exposure, model was put into the photo solidification machine photocuring 40 seconds, resin disk is taken out from model, the back side up, photocuring 40 seconds.Preservation was solidified resin fully in 24 hours and is finished product in dry environment.
Embodiment 2
The nano calcium hydroxide hydrophilic resin that embodiment 1 is obtained and existing three oxidation mineralising polymer (MTA) resins and calcium hydroxide resin compare.Get 30 μ L phenol red solutions (pH=7.0) and drip in three kinds of resin surfaces, observe three kinds of resins keeping the surrounding acid-base value.
Neutral phenol red drips of solution is aubergine on nano calcium hydroxide hydrophilic resin of the present invention surface, illustrates that the nano calcium hydroxide hydrophilic resin has the ability of keeping alkaline environment identical with (MTA) resin, can induce the collagen mineralising in theory.
Embodiment 3:
Nano calcium hydroxide hydrophilic resin, existing (MTA) resin and three kinds of hydrophilic differences of resin of existing calcium hydroxide resin of using contact angle instrument mensuration embodiment 1 to be configured to, sample of the same race is optional gets three, every kind of resin is got three points and is carried out contact angle determination, record the result and use statistics software SPSS11.0 to carry out data statistics, statistical data is as shown in table 1.
Table 1 SPSS11.0 statistical data
Contact angle: 78.5 ± 4.0 degree; Calcium hydroxide resin contact angle: 59.7 ± 2.4 degree; Nano calcium hydroxide resin contact angle: 52.6 ± 3.5 degree.Illustrate that nano calcium hydroxide resin hydrophilic is better than (MTA) resin and calcium hydroxide resin, have significant difference (P＜0.05).
Embodiment 3
Three oxidation mineralising polymers (MTA) group: the simulated body fluid (SBF) that 30 μ L is contained phosphorylation oligochitosan (PCOS) drops in (MTA) hydrophilic resin panel surface, collagen fiber nickel screen face down after sodium tripolyphosphate (TPP) phosphorylation is swum on the drop, placing relative humidity is 100% container mineralising, take out sample when 4 hours and 48 hours respectively, use washed with de-ionized water, drying adopts transmission electron microscope (TEM) to observe and carries out selected area electron diffraction (SEAD) and energy spectrum analysis method (EDS) energy spectrum analysis.
Nano calcium hydroxide hydrophilic resin group: use the nano calcium hydroxide resin disk, mineralising mode and sign are with the experiment of three oxidation mineralising polymers (MTA) group.
(MTA) the resin mineralising is after 12 hours, and mineral is regular to gather around the collagen fiber, and progresses into fibrous inside and formed high density band structure, illustrates that the biomineralization of natural mineralized collagen fiber has taken place to be similar to this collagen.
Nano calcium hydroxide hydrophilic resin mineralising was observed collagen mineralising situation after 48 hours under transmission electron microscope.Mineralized collagen has tangible band structure, illustrates that the biomineralization of natural mineralized collagen fiber has taken place to be similar to this collagen, has produced the classification mineralising in the collagen fiber.
The advantage of calcium hydroxide hydrophilic resin of the present invention:
1, the carious dentin surface shows as demineralization collagen network, intensity reduces, influence bonding force and easily bring out recurrent caries, the collagen remineralization can promote the dentin remineralization and improve the dentin bonding force, therefore how making the collagen remineralization is basic goal of the present invention, the collagen mineralising must realize under the inducing of alkaline environment, nano calcium hydroxide hydrophilic resin of the present invention provides alkaline environment for the collagen mineralising and the calcium ion source is provided, induce collagen generation remineralization, make mineral deposit, the nucleation of crystal, growth more is similar to natural collagen, generation is similar to the band structure of natural collagen in the dentin, improves the mechanical performance of collagen fiber.
Be to allow material be combined with dentin when 2, dental filling material uses, just packing material is prominent embeds in the dentin collagen network structure, in order to improve the prominent packing interaction of packing material, need to improve hydrophilic and the flowability of filler, three kinds of different ratio regular meetings of material produce different Resin Flow and calcium ion slow release effect in the resin, and each component ratio of nano calcium hydroxide hydrophilic resin of the present invention is the ratio that calcium ion slow release and Resin Flow have both.Therefore it had both had the alkaline ability of keeping, and hydrophilic is better than existing (MTA) and calcium hydroxide resin, has better penetration, resin is prominent can more effective embedding collagen network in, improved Dentinal adhesive effect, the length of penetration that more is conducive to calcium ion reaches certain mineralising degree of depth.
3, dental caries decrease surperficial dentin and often can't keep calcium ion concentration and alkaline environment, suppress the collagen remineralization, thereby suppress the dentin remineralization, nano calcium hydroxide hydrophilic resin of the present invention can be kept calcium ion concentration and alkaline environment on every side, can induce the collagen remineralization, thereby inducing the dentin remineralization, is a kind of filler with remineralization ability.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, every foundation technical spirit of the present invention all still belongs in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment does.
Claims (1)
1. calcium hydroxide hydrophilic resin, formed by hydrophilic resin substrate, inorganic filler and the configuration of collagen mineralising derivant, this hydrophilic resin substrate is formed by camphorquinone, 4-(N, N-diformazan ammonia) ethyl benzoate, ethoxy methyl methacrylate and the configuration of bisphenol-A methacrylate ethylene oxidic ester; This inorganic filler is the gas phase nano silicon dioxide of silanization; It is characterized in that the ratio of weight and number of described hydrophilic resin substrate, inorganic filler and collagen mineralising derivant is hydrophilic resin substrate: inorganic filler: collagen mineralising derivant=4: 1: 5; Described collagen mineralising derivant is the nanoscale calcium hydroxide.
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| CN2013102428160A CN103284888A (en) | 2013-06-18 | 2013-06-18 | Calcium hydroxide hydrophilic resin |
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| CN2013102428160A CN103284888A (en) | 2013-06-18 | 2013-06-18 | Calcium hydroxide hydrophilic resin |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791427A (en) * | 2010-01-26 | 2010-08-04 | 南京工业大学 | Alkaline excitation nano silicon dioxide self-curing material with bioactivity and preparation method and application thereof |
| CN102552046A (en) * | 2012-01-13 | 2012-07-11 | 东华大学 | Composite dental restoration resin with silica microspheres as filler and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791427A (en) * | 2010-01-26 | 2010-08-04 | 南京工业大学 | Alkaline excitation nano silicon dioxide self-curing material with bioactivity and preparation method and application thereof |
| CN102552046A (en) * | 2012-01-13 | 2012-07-11 | 东华大学 | Composite dental restoration resin with silica microspheres as filler and preparation method thereof |
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Application publication date: 20130911 |