CN103638042A - Tooth desensitizer as well as preparation method and application thereof - Google Patents

Tooth desensitizer as well as preparation method and application thereof Download PDF

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CN103638042A
CN103638042A CN201310641399.7A CN201310641399A CN103638042A CN 103638042 A CN103638042 A CN 103638042A CN 201310641399 A CN201310641399 A CN 201310641399A CN 103638042 A CN103638042 A CN 103638042A
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mesoporous silica
particle
silica nano
preparation
bioactivity glass
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甘少磊
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Beijing Boenkang Biotechnology Co., Ltd.
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BEIJING BOENKANG BIOTECHNOLOGY Co Ltd
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Abstract

The invention relates to a tooth desensitizer as well as a preparation method and application of the tooth desensitizer. The tooth desensitizer is a powdery composite material, comprises mesoporous silica nano-particles and bioactive glass which is injected into pores of the mesoporous silica nano-particles by fusing. The preparation method of the tooth desensitizer comprises the following steps: (1), providing mesoporous silica nano-particles; (2), providing bioactive glass, wherein the bioactive glass is heated until being fused; (3), immersing the mesoporous silica nano-particles into the fused biological active glass, so that the fused biological active glass is injected into the pores of the mesoporous silica nano-particles; and (4), cooling the mesoporous silica nano-particles which are injected with the bioactive glass to form the powdery tooth desensitizer. The powdery tooth desensitizer disclosed by the invention can be mixed with water to form paste, is coated on a tooth surface with a dentin sensitivity symptom by using a brush, and can deeply seal an exposed dentinal tubule, so that external stimuli in an oral cavity is isolated to achieve effect of treating dentin sensitivity.

Description

Tooth desensitizers, Preparation Method And The Use
Technical field
The present invention relates to a kind of tooth desensitizers, and its production and use.Tooth desensitizers of the present invention can overcome shortcoming of the prior art, the dentinal tubule that more in depth sealing exposes, thus the environmental stimuli in isolated oral cavity reaches the effect for the treatment of dentine hypersensitivity.
Background technology
Dentine hypersensitivity disease mainly causes stimulation to cause because dentinal tubule is exposed in oral environment.The thinking for the treatment of dentine hypersensitivity is broadly divided into two large classes at present: a class is according to neural theory, dentinal fibers conduction theory, adopt potassium-containing compound as the toothpaste of the preparations such as potassium nitrate, potassium chloride or varnish, reduce the sensitivity of Intradental nerve tip, thereby alleviate it for the reaction of environmental stimuli; Equations of The Second Kind is according to hydrodynamic theory, reduces the diameter of dentinal tubule, and the opening of sealing dentinal tubule, reduces Dentinal permeability, to reduce, to avoid the liquid flow in dentin.Equations of The Second Kind method is considered to treat the fundamental way of dentin hypersensitiveness always.
For Equations of The Second Kind method, nano SiO 2 particle due to good biocompatibility, low cost, be easy to be prepared as lower granularity but potential candidate materials.But nano SiO 2 particle is applied to Equations of The Second Kind method and has serious defect: nano SiO 2 particle is immersed in after dentinal tubule, owing to cannot effectively mutually merging and be fixed in dentinal tubule, thereby easily from dentinal tubule, deviate from.Therefore, nano SiO 2 particle is applied in sensitivity of tooth treatment, curative effect is unstable, and the persistent period is short, very easily recurrence.
Bioactivity glass (bioactive glass, BG) is a kind of silicate glass material with special the Nomenclature Composition and Structure of Complexes, by the Hench of Univ Florida USA professor, in 1969, is developed.Bioactivity glass has and osseous tissue formation chemical binding ability, all there is good binding ability with osseous tissue and soft tissue, implant artifact activity glass surface with body fluid generation ionic reaction, finally at glass surface, form the low-crystallinity carbonated hydroxyapatite layer (HCA) of inorganic mineral in similar bone, similar to the skeleton of organism because of chemical composition, it is synostosis that skeleton easily and around forms firmly chemical bonding.Therefore, bioactivity glass is always active in the performance of induced osteogenesis field.Come in, scientist has been found that, bioactivity glass also shows wide prospect in dental care, U.S. biotech firm (U.S. Biomaterials Corporation) has developed the dental materials product of two kinds of bioactivity glass at present, be respectively PerioGlas powder and Nova Min powder, it all shows the good therapeutic effect for periodontal.
But, above-mentioned Equations of The Second Kind method for treatment dentin hypersensitiveness, bioactivity glass does not enter people's the visual field completely, this be because: bioactivity glass is difficult to be prepared as very thin granule, its particle diameter is conventionally the scope of tens microns, yet the diameter of dentinal tubule is only 3~4 μ m at nearly pulp cavity place, and nearly dento enamel junction is only 1 μ m, therefore, bioactivity glass is difficult to enter into dentinal tubule.Therefore, although bioactivity glass has very superior biocompatibility, and there is very positive effect for dental care, temporarily also do not demonstrate and can treat dentin hypersensitiveness by above-mentioned Equations of The Second Kind method.
Therefore, clinically in the urgent need to finding new material, to reach for a long time, to treat efficiently dentine hypersensitivity.
Summary of the invention
The object of the present invention is to provide a kind of tooth desensitizers for the treatment of for a long time, efficiently dentine hypersensitivity, to overcome above-mentioned technical problem of the prior art.
The preparation method of the tooth desensitizers that another object of the present invention is to provide such.
Another object of the present invention is the purposes in the medicine for the preparation for the treatment of sensitivity of tooth that provides such.
The invention provides a kind of tooth desensitizers, it is characterized in that this tooth desensitizers is powdery composite, comprise mesoporous silica nano-particle and by melting, be injected into the bioactivity glass in the hole of described mesoporous silica nano-particle.
The diameter of wherein said mesoporous silica nano-particle is 80nm-150nm, preferred 90nm-140nm, 100nm-130nm, 110nm-120nm, and pore volume is 0.8cm 3/ g-0.9cm 3/ g, preferably 0.81cm 3/ g-0.89cm 3/ g, 0.82cm 3/ g-0.88cm 3/ g, 0.83cm 3/ g-0.87cm 3/ g, and bore dia is 3nm-4nm.
Wherein said tooth desensitizers also comprises the bioactivity glass layer that is coated on described mesoporous silica nano-particle surface by melting.
Wherein the thickness of above-mentioned bioactivity glass layer is 1-30nm, preferably 2-29nm, 3-28nm, 4-27nm, 5-20 nm, 10-20 nm.
Wherein the mass ratio of mesoporous monox nanometer granule and bioactivity glass is (2-4): (0.1-1).
The present invention also provides the preparation method of such tooth desensitizers, comprises
(1) provide mesoporous silica nano-particle,
(2) provide bioactivity glass, to the heating of described bioactivity glass until its melting,
(3) described mesoporous silica nano-particle is immersed in the bioactivity glass of melting, the bioactivity glass of melting is injected in the hole of described mesoporous silica nano-particle,
(4) made to inject the cooling formation powdery of the mesoporous silica nano-particle tooth desensitizers of bioactivity glass.
Wherein said mesoporous silica nano-particle can be according to the method preparation comprising the steps: cetyl trimethyl ammonium bromide, water, sodium hydroxide and ethyl orthosilicate reacts and obtain solid, described solid successively drying and calcine after obtain described mesoporous silica nano-particle.
The mol ratio of wherein said cetyl trimethyl ammonium bromide, water, sodium hydroxide and ethyl orthosilicate is 1:(4895-9719): (2-3): (4.88-11.38), preferred 1:(4895-8504): (2-2.55): (4.88-8.13).
Wherein, in preparing mesoporous silica nano-particle process, reaction temperature can be 65 ℃-75 ℃, as 70 ℃; Response time can be 1.5 hours-4 hours, as 2 hours; Baking temperature can be 50 ℃-70 ℃, as 50 ℃; Can be 6 hours drying time-24 hours, as 10 hours; The temperature of described calcining can be 500 ℃-600 ℃, as 550 ℃; The time of described calcining can be 4 hours-8 hours, as 4 hours.
Wherein the melt temperature in step (2) is 1200-1500 ℃, preferably 1300-1400 ℃.
Wherein the immersion time in step (3) is 10 seconds to 5 minutes, preferably 1-4 minute.
The invention still further relates to the purposes of above-mentioned tooth desensitizers in the medicine for the preparation for the treatment of sensitivity of tooth.
The tooth desensitizers that said method of the present invention provides can mix to form with water paste, available medical little brush is evenly applied in the Tooth surface of suffering from dentine hypersensitivity symptom subsequently, can repeat to smear 3~5 times, wait for after 15 minutes, this composite completes curing, the dentinal tubule that more in depth sealing exposes, thus the environmental stimuli in isolated oral cavity reaches the effect for the treatment of dentine hypersensitivity.
In hole due to mesoporous silica nano-particle of the present invention, injected and on bioactivity glass and/or surface, be coated bioactivity glass layer, when mesoporous silica nano-particle enters after dentinal tubule, this bioactivity glass can discharge calcium ion and phosphate anion, the calcium ion that these discharge and the phosphate anion gap between mesoporous silica nano-particle is in conjunction with also crystallization, thereby mesoporous silica nano-particle is bonded together with stable being present in dentinal tubule, this has overcome the problem that silica dioxide granule is easily deviate from from dentinal tubule, can be long-term, treat efficiently dentine hypersensitivity.And, bioactivity glass itself has very excellent biocompatibility, this makes the tooth desensitizers of the present invention can be extraordinary compatible with human body, while bioactivity glass itself or good dental care material, particularly, in the treatment of periodontal, therefore, tooth desensitizers of the present invention is when can treating dentine hypersensitivity efficiently, can also effectively prevent and treat other oral disease, particularly periodontal.This makes tooth desensitizers of the present invention have boundless market prospect.
 
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) and transmission electron microscope (TEM) characterization result of the mesoporous silica nano-particle of preparation in embodiment 1; Wherein, the photo that Fig. 1 (a) is scanning electron microscope, the photo that Fig. 1 (b) is transmission electron microscope.
Fig. 2 is the characterization result of the little angle X x ray diffraction (little angle XRD) of the mesoporous silica nano-particle of preparation in embodiment 1.
Fig. 3 is the laser co-focusing characterization result of having sealed the mesoporous silica nano-particle of fluorescent dye in embodiment 1.
Fig. 4 injects the SEM morphology characterization result after bioactivity glass in the mesoporous silica nano-particle of preparing in embodiment 1.
Fig. 5 is the TEM characterization result of the mesoporous silica nano-particle surface coated biologically active glassy layer of preparation in embodiment 1.
Fig. 6 is the SEM of dental disk and power spectrum test after coating composite materials in embodiment 1; Wherein, the dental disk surface that Fig. 6 (a) is uncoated composite; Fig. 6 (b) is the dental disk surface after coating composite materials; The impression of the Yi Ge dentinal tubule that Fig. 6 (c) blocks for coated material; Fig. 6 (d) is the power spectrum result at Hei Quan position in Fig. 6 (c); Fig. 6 (e) and Fig. 6 (f) were for applying the dental disk cross-section morphology of composite.
Fig. 7 is the SEM characterization result of the mesoporous silica nano-particle of preparation in embodiment 2
Fig. 8 is the SEM characterization result of the mesoporous silica nano-particle of preparation in embodiment 3.
Fig. 9 injects the SEM morphology characterization result after bioactivity glass in the mesoporous silica nano-particle of preparing in embodiment 2.
Figure 10 injects the SEM morphology characterization result after bioactivity glass in the mesoporous silica nano-particle of preparing in embodiment 3.
 
The specific embodiment
The test method that following embodiment is used if no special instructions, is known conventional method
The material using in following embodiment, reagent etc., if no special instructions, all commercially available acquisitions.
 
Embodiment 1
(1) preparation of mesoporous silica nano-particle
Proportioning raw materials is cetyl trimethyl ammonium bromide (CTAB): deionized water: sodium hydroxide: ethyl orthosilicate (TEOS)=1: 8504: 2.55: 8.13 (mol ratios); According to said ratio, mix cetyl trimethyl ammonium bromide, deionized water and sodium hydroxide, reaction system is stirred to temperature stabilization in 70 ℃, and after cetyl trimethyl ammonium bromide dissolves completely, drips fast ethyl orthosilicate; Reaction system remains on 70 ℃ of reactions 2 hours, and after completion of the reaction, sucking filtration obtains white solid dries 10 hours at 50 ℃, baking oven; Resulting white powder sample is ground with mortar, put into crucible, 550 ℃ of calcinings of Muffle furnace 4 hours, remove template CTAB; Sample after calcining is porphyrize again, obtains having the mesoporous silica nano-particle in orderly duct, and pore volume is 0.84cm3/g, and bore dia is 3.0nm;
The scanning of mesoporous silica nano-particle and transmission electron microscope characterization result as shown in Fig. 1, from SEM result, the mesoporous silica nano-particle size of preparation between 120~150nm, pattern almost spherical, uniformity is better.In TEM photo, can see nano particle ordered mesopore orbit, the striped in figure on granule is the clear opening duct being arranged in parallel, and such duct is conducive to load and discharge molecule.
The little angle X optical diffraction characterization result of mesoporous silica nano-particle has proved the good order of this material, as shown in Fig. 2, in figure, abscissa is 2 θ angles, vertical coordinate is that peak is strong, can see that 2 ° are located typical mesoporous peak, simultaneously because material order is better, can see multistage diffraction maximum, stronger in figure have 3 grades of peaks, at 6 °, locates to also have 4 grades of weak peaks.
As shown in Fig. 3, this mesoporous silica nano-particle is smeared by surface the degree of depth that can infiltrate dentinal tubule and is characterized by laser co-focusing.In figure, arrow is depicted as the application side of material, can see the sample border of an inclination.Red light is that the rhodamine B dyestuff of sealing in mesoporous SiO 2 granule excites, its labelling the position of mesoporous silicon sphere, therefore the degree of depth that red area can reach has shown material accessible degree of depth in dentinal tubule, bosom can reach 160 microns, laser high light, generally infiltrates and reaches 110 microns.
(2) melting of bioactivity glass
Bioactivity glass purchased from Shanghai Guijian Biological Material Co., Ltd. is heated to 1200 ℃ and makes its melting.
(3) mesoporous silica nano-particle is immersed in the bioactivity glass of melting to 2 minutes, so that the bioactivity glass of melting is injected in the hole of mesoporous silica nano-particle.The mesoporous silica nano-particle that has injected bioactivity glass in hole is cooling and reclaim to obtain powdery composite, i.e. tooth desensitizers in the present invention.
The pattern of mesoporous silica nano-particle that has injected the bio-vitric of melting in the hole of above-mentioned preparation characterizes by scanning electron microscope, and it is presented in Fig. 4.Material granule regular shape degree declines, but still can be observed obvious spheroidal particle.
(4) tooth desensitizers of above-mentioned preparation is used to autoclave sterilization (concrete sterilization conditions is that pressure maintains the lower 126 ℃ of sterilizings of 0.15MPa 20 minutes); Tooth desensitizers after sterilization is added to distilled water (mass ratio of tooth desensitizers and distilled water is 2: 3), can with medical little spoon and Liquid dropping bottle, measure fast respectively, the material paste that is white in color after evenly mixing, is the material that can treat dentine hypersensitivity; Using method is as follows: with medical little brush, this white mixture is evenly applied in to tooth surface and (uses medical 17% EDTA solution cleaning dental surface chip, clear water after rinsing blots dental surface moisture), repeat to smear, repeatedly after three times, wait for 15 minutes so that material solidification, this process is noted immediately clearing up saliva of buccal cavity with utensil.
For the sign of this clogged with material dentinal tubule effect, method of testing is: tooth sample is polished off after enamel, perpendicular to jaw gum direction, get the dental disk that dentin part machine cuts into 1mm; Dental disk is put into 17% EDTA solution and is soaked 5 minutes, removes chip, with suck dry moisture after washed with de-ionized water; Go the material of above-mentioned preparation to be evenly applied in the upper surface (away from a side of pulp cavity) of dental disk sample, with filter paper, sop up surperficial residual materials after slightly dry, repeat to smear, repeatedly after three times, dry and within 15 minutes, treat material solidification; After solidifying, section is put into deionized water and clean, with little brush, brush away gently the unnecessary material in surface, dry, fasten with glue on SEM sample stage, after metal spraying, carry out SEM observation.
The SEM characterization result of materials'use effect is as shown in Fig. 6: wherein, the front surface of the dentinal tubule of uncoated material as shown in Fig. 6 (a), smooth surface, the dentinal tubule of hole, tubulose hole for exposing, diameter is in 3 μ m left and right.Fig. 6 (b) is for smearing the state of dentin surface after material, linen impression is material and blocks the vestige after dentinal tubule, but integral body is seen, in its surface and Fig. 6 (a), the smooth surface of uncoated material is also had any different, here can see significantly layer of material coat, but whole quality is finer and smoother, there is no bulky grain calcium phosphate aqueous solution salt crystal accumulation in surface, this is after material solidification, with medical brush, to scrub gently the result on surface, also illustrated that material is after the setting time of 15 minutes simultaneously, better with Dentinal adhesiveness, can't be because of again being washed away by water and coming off.Rapid solidification, adhesiveness are good, and this is all the important investigation index to material in clinical practice.
Fig. 6 (c) is the enlarged drawing of a blocked tubule, can see that this layer of coat consists of many fine particles after amplification more clearlyly.These fine particles had both derived from body of material part-mesoporous silica nano-particle, meanwhile, thereby be again the calcium ion that discharges of bioactivity glass and phosphate anion in conjunction with and crystallize into the result that calcium phosphate combines mesoporous silica particles.Cause is the Electronic Speculum test result from Fig. 1, the diameter of simple mesoporous silica nano-particle is only between 120~150nm, be less than the granule of observing in Fig. 6 (c), therefore can infer, be that calcium phosphate crystal adheres to each other a plurality of mesoporous particles to have formed larger granule like this.In fact, examine between the granule in photo, also have the vestige of " bonding cement " existence being formed by calcium phosphate crystal.This makes the mesoporous silica nano-particle can very firm, permanent being present in dentinal tubule.
Fig. 6 (d) is the power spectrum test of black circle mark in Fig. 6 (c), wherein silicon Si is the peculiar element of mesoporous silica nano-particle, phosphorus P and calcium Ca are except the calcium ion and phosphate anion that discharge from bioactivity glass, dentin also consists of calcium phosphate, therefore these two kinds of constituent contents are higher, and golden Au is that in SEM sample preparation process, metal spraying is introduced.The result of this power spectrum test has proved that the material that is blocked in dentinal tubule's mouth is our prepared mesoporous material really.
Fig. 6 (e) and (f) be the sectional drawing of dental disk after breaking into two with one's hands.In Fig. 6 (e), can be observed and manage a surface topography for the diverse dentinal tubule of dentin, depth of field degree by SEM judges, dentinal tubule non-NULL, but be filled material, particularly, near the existence of a spherical impression of pipe centre, the surface topography that this and non-natural have is described.And the pattern that enters the implant between pipe conforms to the material pattern that is coated on dentin surface in Fig. 6 (c).Therefore judge that the mesoporous silica nano-particle that has injected melting bio-vitric has been deep among dentinal tubule, complement one another and prove with laser co-focusing result.
Fig. 6 (f) is that material is along with the increase (from left to right) of depth of penetration, gradually by completely to empty transition, increase due to amplification, material pattern is more clear, can see that between its apparent pattern of the fuller material of packing ratio and pipe, dentin has certain similarity, but granule is more tiny a little, meanwhile, fills more empty part and also can see the existence of some spheroidal particle.This is by completely showing that to empty transition the infiltration of material is close to dentinal tubule tube wall and flows into, and this is the coefficient result of surface tension and adhesiveness.The material using clinically now, infiltrate dentinal tubule and solidify after and between tube wall, there will be obvious gap, in conjunction with defective tightness, but in the observation of the sample of the lot of materials result of use of carrying out at us, and similar state appears in none example, it is very closely that visible this material is combined with tube wall.This closely in conjunction with making tooth desensitizers of the present invention can treat for a long time, efficiently dentine hypersensitivity.
 
Embodiment 2
(1) preparation of mesoporous silica nano-particle
Proportioning raw materials is cetyl trimethyl ammonium bromide (CTAB): deionized water: sodium hydroxide: ethyl orthosilicate (TEOS)=1: 4859: 2: 8.13 (mol ratios); According to said ratio, mix cetyl trimethyl ammonium bromide, deionized water and sodium hydroxide, reaction system is stirred to temperature stabilization in 70 ℃, and after cetyl trimethyl ammonium bromide dissolves completely, drips fast ethyl orthosilicate; Reaction system remains on 70 ℃ of reactions 2 hours, and after completion of the reaction, sucking filtration obtains white solid dries 10 hours at 50 ℃, baking oven; Resulting white powder sample is ground with mortar, put into crucible, 550 ℃ of calcinings of Muffle furnace 4 hours, remove template CTAB; Sample after calcining is porphyrize again, obtains having the mesoporous silica nano-particle in orderly duct, and pore volume is 0.89cm3/g, and bore dia is 3.0nm;
As shown in Figure 7, particle size enlarges markedly than the granule in embodiment 1 the scanning electron microscope characterization result of mesoporous silica nano-particle, and uniformity reduces, and size particles size differs larger, but still can keep the shape of almost spherical.
(2) melting of bioactivity glass
Bioactivity glass purchased from Shanghai Guijian Biological Material Co., Ltd. is heated to 1500 ℃ and makes its melting.
(3) mesoporous silica nano-particle is immersed in to 10 seconds in the bioactivity glass of melting, so that the bioactivity glass of melting is injected in the hole of mesoporous silica nano-particle.The mesoporous silica nano-particle that has injected bioactivity glass in hole is cooling and reclaim to obtain powdery composite, i.e. tooth desensitizers in the present invention.
The pattern of mesoporous silica nano-particle that has injected the bio-vitric of melting in the hole of above-mentioned preparation characterizes by scanning electron microscope, and it is presented in Fig. 9.Material granule regular shape degree declines, but still can be observed obvious spheroidal particle.
The tooth desensitizers of above-mentioned preparation is used to autoclave sterilization (concrete sterilization conditions is that pressure maintains the lower 126 ℃ of sterilizings of 0.15MPa 20 minutes); Tooth desensitizers after sterilization is added to distilled water (mass ratio of tooth desensitizers and distilled water is 3: 4.5), can with medical little spoon and Liquid dropping bottle, measure fast respectively, the material paste that is white in color after evenly mixing, is the composite that can treat dentine hypersensitivity.
 
Embodiment 3:
(1) preparation of mesoporous silica nano-particle
Proportioning raw materials is cetyl trimethyl ammonium bromide (CTAB): deionized water: sodium hydroxide: ethyl orthosilicate (TEOS)=1: 9719: 2.55: 8.13 (mol ratios); According to said ratio, mix cetyl trimethyl ammonium bromide, deionized water and sodium hydroxide, reaction system is stirred to temperature stabilization in 70 ℃, and after cetyl trimethyl ammonium bromide dissolves completely, drips fast ethyl orthosilicate; Reaction system remains on 70 ℃ of reactions 2 hours, and after completion of the reaction, sucking filtration obtains white solid dries 10 hours at 50 ℃, baking oven; Resulting white powder sample is ground with mortar, put into crucible, 550 ℃ of calcinings of Muffle furnace 4 hours, remove template CTAB; Sample after calcining is porphyrize again, obtains having the mesoporous silica nano-particle in orderly duct, and pore volume is 0.81cm 3/ g, bore dia is 3.0nm;
As shown in Figure 8, particle size is less than the granule in embodiment 1 for the scanning electron microscope characterization result of mesoporous silica nano-particle, but uniformity and dispersibility are lower slightly, and granule still can keep the shape of almost spherical
(2) melting of bioactivity glass
Bioactivity glass purchased from Shanghai Guijian Biological Material Co., Ltd. is heated to 1350 ℃ and makes its melting.
(3) mesoporous silica nano-particle is immersed in the bioactivity glass of melting to 5 minutes, so that the bioactivity glass of melting is injected in the hole of mesoporous silica nano-particle.The mesoporous silica nano-particle that has injected bioactivity glass in hole is cooling and reclaim to obtain powdery composite, i.e. tooth desensitizers in the present invention.
The pattern of mesoporous silica nano-particle that has injected the bio-vitric of melting in the hole of above-mentioned preparation characterizes by scanning electron microscope, and it is presented in Figure 10.Material granule regular shape degree declines, but still can be observed obvious spheroidal particle.
The tooth desensitizers of above-mentioned preparation is used to autoclave sterilization (concrete sterilization conditions is that pressure maintains the lower 126 ℃ of sterilizings of 0.15MPa 20 minutes); Tooth desensitizers after sterilization is added to distilled water (mass ratio of tooth desensitizers and distilled water is 2: 3), can with medical little spoon and Liquid dropping bottle, measure fast respectively, the material paste that is white in color after evenly mixing, is the composite that can treat dentine hypersensitivity.
 
From the result of the test of above-described embodiment, can clearly find out, it is very closely that the tooth desensitizers in the present invention is combined with dentinal tubule wall, this closely in conjunction with making tooth desensitizers of the present invention can treat for a long time, efficiently dentine hypersensitivity.Bioactivity glass itself has very excellent biocompatibility simultaneously, this makes the tooth desensitizers of the present invention can be extraordinary compatible with human body, and bioactivity glass itself or good dental care material, particularly in the treatment of periodontal, therefore, tooth desensitizers of the present invention can, efficiently treat dentine hypersensitivity in, can also effectively prevent and treat other oral disease, particularly periodontal.This makes tooth desensitizers of the present invention have boundless market prospect.

Claims (12)

1. tooth desensitizers, is characterized in that this tooth desensitizers is powdery composite, comprises mesoporous silica nano-particle and by melting, is injected into the bioactivity glass in the hole of described mesoporous silica nano-particle.
2. the tooth desensitizers of claim 1, the diameter that it is characterized in that described mesoporous silica nano-particle is 80nm-150nm, pore volume is 0.8cm 3/ g-0.9cm 3/ g and bore dia are 3nm-4nm.
3. claim 1 or 2 tooth desensitizers, is characterized in that described tooth desensitizers also comprises the bioactivity glass layer that is coated on described mesoporous silica nano-particle surface by melting.
4. the tooth desensitizers of claim 3, the thickness that it is characterized in that described bioactivity glass layer is 1-30nm.
5. the tooth desensitizers of any one in claim 1-4, the mass ratio that it is characterized in that mesoporous monox nanometer granule and bioactivity glass is (2-4): (0.1-1).
6. the preparation method of the tooth desensitizers of any one in claim 1-5, comprises
(1) provide mesoporous silica nano-particle,
(2) provide bioactivity glass, to the heating of described bioactivity glass until its melting,
(3) described mesoporous silica nano-particle is immersed in the bioactivity glass of melting, the bioactivity glass of melting is injected in the hole of described mesoporous silica nano-particle,
(4) made to inject the cooling formation powdery of the mesoporous silica nano-particle tooth desensitizers of bioactivity glass.
7. the preparation method of claim 6, it is characterized in that described mesoporous silica nano-particle is according to the method preparation comprising the steps: cetyl trimethyl ammonium bromide, water, sodium hydroxide and ethyl orthosilicate reacts and obtain solid, described solid successively drying and calcine after obtain described mesoporous silica nano-particle.
8. the preparation method of claim 7, the mol ratio that it is characterized in that described cetyl trimethyl ammonium bromide, water, sodium hydroxide and ethyl orthosilicate is 1:(4895-9719): (2-3): (4.88-11.38).
9. claim 6 or 7 preparation method, is characterized in that in preparing mesoporous silica nano-particle process, and reaction temperature is 65 ℃-75 ℃; Response time is 1.5 hours-4 hours; Baking temperature is 50 ℃-70 ℃; Be 6 hours-24 hours drying time; The temperature of described calcining is 500 ℃-600 ℃; The time of described calcining is 4 hours-8 hours.
10. the preparation method of any one in claim 6-9, is characterized in that the melt temperature in step (2) is 1200-1500 ℃.
The preparation method of any one in 11. claim 6-10, is characterized in that the immersion time in step (3) is 10 seconds to 5 minutes.
The purposes of the tooth desensitizers of any one in the medicine for the preparation for the treatment of sensitivity of tooth in 12. claim 1-5.
CN201310641399.7A 2013-12-04 2013-12-04 Tooth desensitizer as well as preparation method and application thereof Pending CN103638042A (en)

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CN104825542A (en) * 2015-04-23 2015-08-12 广西达庆生物科技有限公司 Medical biological tooth desensitizer dressing and preparation method thereof
CN104860539A (en) * 2015-04-16 2015-08-26 南京众力盛强新材料科技有限公司 Mesoporous silicon oxide ceramic composite material and preparation method thereof
CN108186614A (en) * 2018-02-22 2018-06-22 南京医科大学附属口腔医院 A kind of bioactivity glass composite membrane, preparation method and application
CN108618967A (en) * 2018-05-29 2018-10-09 中国科学院化学研究所 A kind of tooth desensitizers and its preparation method and application containing phosphosilicate glass
CN109820735A (en) * 2019-03-14 2019-05-31 东华大学 A kind of porous SiO of dendroid2Base compound resin and its preparation and application
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CN109820735A (en) * 2019-03-14 2019-05-31 东华大学 A kind of porous SiO of dendroid2Base compound resin and its preparation and application
CN113827492A (en) * 2021-11-29 2021-12-24 诺一迈尔(山东)医学科技有限公司 Tooth desensitizing composition and preparation method thereof

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