CN107648055B - A kind of sodium fluoride anticaries tooth plastics and preparation method thereof - Google Patents
A kind of sodium fluoride anticaries tooth plastics and preparation method thereof Download PDFInfo
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- CN107648055B CN107648055B CN201710912119.XA CN201710912119A CN107648055B CN 107648055 B CN107648055 B CN 107648055B CN 201710912119 A CN201710912119 A CN 201710912119A CN 107648055 B CN107648055 B CN 107648055B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/20—Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
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Abstract
A kind of sodium fluoride anticaries tooth plastics and preparation method thereof are disclosed, the sodium fluoride anticaries tooth plastics include following component in parts by weight：Sodium fluoride 50 450, rosin 1,000 3200, frankincense 150 430, acrylic resin 200 450,95% ethyl alcohol, 1200 2000g.Film made from the plastics is strong to tooth adhesion, and can slow release fluoride to avoid fluoride acute poisoning and keep it is long-acting, and have good appearance.
Description
Technical field
The present invention relates to a kind of sodium fluoride anticaries tooth plastics and preparation method thereof.
Background technology
Dental caries are the infection that the chronic progressive that dental hard tissue occurs under the multifactor effect based on bacterium destroys
Property disease, illness rate is high, damaging range is wide.China's third time oral healthy condition epidemiological survey is shown：The 5 years old youngster in China
The illness rate of virgin caries in primary teeth is that 66.0%, 35-44 Sui a middle-aged person's dental caries illness rate is 88.1%, 65-74 Sui the elderly's dental caries
Sick illness rate may be up to 98.4%.The early stage of dental caries only has the demineralization and discoloration of enamel.When lesion is further to Deep Development, then
It can lead to the defect of tooth, while have the symptoms such as sensitivity, pain, it might even be possible to cause pulpitis, periapical inflammation and jaw bones
The complications such as marrow inflammation；More severe patient can cause loss of tooth, denture defect etc., to which the whole body for influencing feed and body is strong
Health.Therefore, early treatment dental caries are particularly significant for reducing defect of teeth, mitigating patient suffering and prevent complication
's.
Clinically have at present to the therapy of incipient dental caries：Piece cuts, abrade demineralization or enamel that dental caries are bad, plombage or applies nitre
Sour silver etc..These methods such or such make it be restricted in clinical application due to all there is a problem of.For example, piece cut and
Enamel and tooth structure and shape can be damaged after abrading tissue of tooth, easily leads to the generation of secondary caries；And filling treatment then must
Abrade more normal tissue of tooth, while aging, the discoloration of obturation will influence filling effect, obturation and tissue of tooth it
Between existing Micro blazed-grating phenomenon, the formation of secondary caries can be caused；And application of silver nitrate then stops the bad development of dental caries, lesion cannot be made to repair
It is multiple, and can cause tooth discoloration that patient is made to be difficult to receive.The purpose for the treatment of is to cure, and above-mentioned therapy is only in certain journey
Achieve the purpose that treatment on degree, and far from healing.In addition, for occur during correction the hickie formed due to acid etching,
The sensitivity etc. that the early stage neck portion demineralization of neck portion wedge type defect generates there is no effective therapy at present.Therefore, one is found
The new anti-dental caries product of kind seems very necessary.
20th century, medical circle of oral cavity be found that fluoride can anticaries, by the exploration of decades, research, fluorination
Object preventing decayed tooth technology has obtained WHO and the authoritative institution of many countries is recommended, and is able to worldwide extensive use.It is common pre-
The means of anti-caries have：Fluorination drinking-water, using toothpaste with fluoride and mouthwash, using fluorine film and fluorine gel, fissure blockade and change
Good diet etc., domestic market fluoride preparation have fluoride gel (main component：Sodium fluoride, potassium chloride, calcium chloride, phosphoric acid) and fluorine-containing bubble
Foam (main component：Acid fluorophosphate, thickener, fluorine ion stabilizer, foaming agent, sugar element, essence are equipped with disposable denture fixing device
Shape：When standing the foam that nozzle sprays white dense is pressed for transparent liquid hand) etc., many fluoride preparation generally existings：With tooth enamel
The binding ability on matter surface is poor, in oral cavity existence time it is short and use when it is inconvenient the problems such as.
In the local fluoride in caries prevention measure of clinical application at present, fluoride varnish is practical with it, effective, safe, is easy to grasp
Make, the advantages that patient is easy to receive, best fluoride preventing decayed tooth mode be described as by WHO, be at present in the world it is most widely used, most have
The preventing decayed tooth means of effect.Fluoride varnish is a kind of lower fluorine-containing dental material of novel concentration, is the one kind for being coated on facing
Protective coating, main component are fluorides, also contain a little beeswax etc. and flow the ingredients such as thickener and sweetener, the production
Product come across the 1960s and 1970s, quickly grow in recent years.
CN103961266B discloses a kind of nanometer of carboxymethyl chitosan sodium fluoride anticaries film and preparation method thereof and answers
With the nanometer carboxymethyl chitosan fluoride film is by special with drug slow release function, biocidal property and biocompatibility etc.
Property nanometer carboxymethyl chitosan particle and generated from acid etching resin adhesive and corresponding fluoride with light-cured performance；
Carboxymethyl chitosan is first prepared into nanoparticle, sodium alginate soln is added in the forming process of nanoparticle, to promote shape
At the nano particle of centralized particle diameter.
CN105496797A discloses a kind of photocuring preventing decayed tooth fluoride film, it is characterised in that：Its by ingredient A and at
Divide B compositions；The group of the ingredient A becomes：Bis-GMA：15wt%HEMA：35wt%4-ME T：8wt% sodium fluorides：10wt%
CB-1：10.5wt% camphorquinones：0.05wt% sodium carboxymethylcelluloses：10wt% colloidal silicon dioxides：Surplus is to 100wt%；
The group of the ingredient B becomes：Bis-GMA：50wt%, TEGDMA：25wt%, DMAEMA：0.03wt%, p-TSNa：
0.03wt%, colloidal silicon dioxide：Surplus is to 100wt%.
CN103356399A disclose it is a kind of can pre- anti-caries toothpaste, including rubbing agent, washing foam agent, adhesive,
Moisturizer, sweetener, aromatic further include the fluorination with lotion mass ratio for 2%-5% aleurones enzyme, 1.2%-1.5%
The zinc fluoride of sodium, 2%-3.6%.
CN103417399A discloses a kind of toothpaste with fluoride, is made of by weight percentage following components：0.6-1.2%
Sodium monofluorophosphate, 0.1-0.3% sodium fluorides, 45-55% calcium carbonate, 10-14% glycerine, 16-20% sorbierites, 1-2% Guars
Glue, 0.2-0.6% magnesium monohydrogen phosphates, 1.8-2.6% lauroyl both sexes base disodium beclomethasones, 1-3% whitening agents, surplus is water；Institute
Whitening agent is stated to be made of by weight following components：40-60 parts of sodium phytates, 10-20 parts of aloins, 10-20 portions of Radix Glycyrrhizaes
Glucin and 15-25 parts of glucose oxidases.
CN101502647A discloses a kind of pharmaceutical composition prevented or/and treat saprodontia, it is by dextranase
It is prepared for active constituent with sodium fluoride, wherein containing NaF-10-80 μ g, dextranase 1-4U in every milliliter, also provides
The preparation method of the pharmaceutical composition, the drug are the sodium fluoride and Dex use in conjunction that will be less than clinical dosage, reduce fluorine
The dosage for changing sodium can play the role of inhibiting plaque bio-film in its subinhibitory concentration
JP2001-056011A discloses dietary composition and oral cavity composition with anti-dental caries function, the composition
Including chondroitin sulfate oligosaccharides, the composition includes the buffer for having in the oral cavity pH cushioning effects.
WO2010/075419A1 discloses a kind of composition for reducing teeth demineralization and promoting remineralization, institute
It includes the combination with the following terms to state composition：A) a kind of chlorine dioxide source；B) a kind of fluoride sources；And a kind of c) buffering
Agent.
" sodium fluoride film is in the application for preventing correction tooth demineralization ", Feng Huifen etc., international medical and health Leader, 2012,18
(2):157-159 discloses effect of the fluoride film in terms of preventing decayed tooth and prevention, reduction and prevention enamel decalcification, test
Method is 68 malocclusion patients of selection, is equably coated with sodium fluoride film around the bracket on facing with small brushes, with
Every three months even spread 1 time afterwards, case tracing study 1 year find patient's demineralization rate 25% after coating sodium fluoride film, fluorination
Sodium film has good result in terms of preventing correction enamel decalcification.
In summary, the effect to fluoride product and mechanism all compare approval both at home and abroad at present.However, in existing fluorine
It is grasped when in compound product, that there are the binding abilities of plastics and enamel surface is poor, existence time is short in oral cavity and use
Make the problems such as inconvenience, and the release of fluoride is uneven, this is seriously restricted its application.This field needs a kind of and tooth
It is the binding ability of enamel surfaces and existence time is grown in oral cavity use, easy to operate and with fluorine long-acting slow-release function
Sodium fluoride anticaries tooth plastics.
Invention content
To solve the above-mentioned technical problems in the prior art simultaneously, the present invention provides a kind of paintings of sodium fluoride anticaries tooth
Film, the plastics include following component in parts by weight or its to prepare raw material include following component in parts by weight：
Preferably, the plastics also include the river wax of 2-10 parts by weight.
Preferably, the plastics also include the colloidal silicon dioxide of 2-10 parts by weight.
In a preferred embodiment of the present invention, the plastics also include the lemon triethylenetetraminehexaacetic acid of 10-45 parts by weight
Ester.
In a preferred embodiment of the present invention, which also includes suitable sweetener and/or essential oil.This
Field technology personnel can determine its content according to the requirement of sugariness and fragrance.
For the present invention, the total weight parts of the plastics can be 5000 parts.
It is highly preferred that the average grain diameter of sodium fluoride is 2-40 μm, preferably 5-20 μm in the plastics.
It is highly preferred that the sodium fluoride is the crystal grain with face-centred cubic structure.
The present inventor it has been investigated that, plastics are strong and weak to the adhesive force of tooth and the sustained release of fluorine is extremely important, fluorination
Object film is covered in dental surface in the form of emulsion paint, cures after encountering saliva and maintains to be present in dental surface, if solidification
Time is too short or too long, can all influence homogenization degree, causes ineffective.Therefore, it is necessary to be studied by formulation and technology, make it
Through suitable hardening time, at least up to performance indicator similar in reference product.In addition, fluoride film must slow release
Just it is avoided that fluoride acute poisoning.The present invention above-mentioned formula can release fluoride and hardening time it is reasonable.
The present inventor has found that the pattern and purity of sodium fluoride particle not only influence made fluoride after further study
The stability of suspension, and then the adhesive ability of plastics is influenced, also affect the sustained release of sodium fluoride, particularly fluorine ion.
In the prior art, influence of the sodium fluoride pattern to plastics adhesive force and sustained release process is usually ignored, research is concentrated mainly on
In the selection of filmogen.For this purpose, the present inventor passes through numerous studies, a kind of sodium fluoride, particularly fluorination sodium crystal are provided
Preparation method, the sodium fluoride that this method obtains makes plastics obtained have good adhesive ability and fluorine ion sustained release effect
Fruit.The method may include following steps：
(1) in batch reactor, loading ammonium fluoride solution reaches about half of reactor volume, then uses pump by hydrogen-oxygen
Change sodium solution to be continuously added in reactor, sodium hydroxide solution feeding line is close to reactor wall and it is exported and blender
Impeller tips horizontal aligument；
(2) continue to feed sodium hydroxide solution until reactor is filled into its final swept volume, sodium hydroxide solution into
The time that material reaches needed for the final working volume of reactor is known as feed time, and feed time was controlled at 60-90 minutes；
(3) after addition of the sodium hydroxide solution, gained suspension is taken out, is transferred in autoclave, is pressed in 5-10MPa
Hydro-thermal process 6-12 hours, is not stirred during hydro-thermal at a temperature of power and 80-120 DEG C；
(4) it will filter in reaction system vacuum after hydro-thermal, washed with ethanol solution, obtain fluorination sodium crystal.
Preferably, in step (1), a diameter of 2-4mm of the feeding line, preferably 3mm.
Preferably, in step (1), the reactant concentration of ammonium fluoride and sodium hydroxide is 0.30- independently of one another
3.50mol/L, preferably 0.40-1.0mol/L.
Preferably, step (1) carries out at a temperature of 20-50 DEG C.
The present inventor it has been investigated that, when by sodium hydroxide solution inject reactor to induce sodium fluoride to crystallize when, reaction
Solution in device is initially clear state, this is because the degree of supersaturation of sodium fluoride is too low and postpones, then as charging into
Row since the degree of supersaturation of solution reaches the critical level of primary nucleation, and then makes solution since crystallization generates crystallization bath foam
Become muddy suddenly.Hereafter, degree of supersaturation is maintained at low-level, because the increase of degree of supersaturation caused by reaction is all given birth to by crystal
Length is consumed, and secondary nucleation is generated, and secondary nucleation is very important crystal nucleation, is crystallized in the sodium fluoride of the present invention
In, it control feed time and is stirred position and ensures secondary nucleation, the control of the low degree of supersaturation after initial initial nucleation
System ensures secondary nucleation well again, ensures that preferable sodium fluoride grain morphology.
The present inventor also found that after secondary nucleation, actually there are still certain defects (such as Fig. 2 institutes for crystal grain through research
Show), therefore the present invention is handled using follow-up hydrothermal, so that crystal form is become regular (as shown in Figure 1), this still belongs to reports for the first time.From
And the sodium fluoride crystal grain of acquisition is enable to be particularly useful for anti-caries plastics of the invention.
Acrylic resin as one of film forming agent is equally important to the performance of plastics.For the present invention, institute
It is preferably the acrylic resin containing repetitive unit shown in lower formula (I) to state acrylic resin：
The number-average molecular weight of the acrylic resin is preferably 300-10000, more preferable 500-8000, most preferably
1000-5000。
The acrylic resin is preferably made by the following method：In N2Under atmosphere, in the toluene as solvent, use
AIBN (2.0wt% of total reaction mixture) is used as initiator, make silicon-containing monomer (SiM) and methacrylic acid monomer (MMA) in
Carried out at 100-110 DEG C reaction 1-3 hours, after the completion of reaction, reaction mixture is cooled down at room temperature, by resin it is cold oneself
It precipitates and filters in alkane (0-2 DEG C), then resin is dried under vacuum to constant weight 10-20 hours at 20-30 DEG C, obtained opaque
White powder, the as described acrylic resin.
This method is simple, efficient, and the acrylate purity obtained is high, and molecular weight is in Unimodal Distribution.
In the method, it is preferable that the polymerisation be equipped with blender, return-flow system, temperature control system, plus
Hot jacket and N2It is carried out in the glass reactor of gas access-outlet system.
In the method, it is preferable that the molar ratio of SiM/MMA is preferably 1.0:0.8 to 0.8:1.0.Certainly, this field
Technical staff is it can be appreciated that the molar ratio of SiM/MMA can also be 1:3-3:1, there are different repeat units to can get
The acrylic resin of ratio.
The silicon-containing monomer (SiM) is such as shown in following formula (II)：
The silicon-containing monomer can be easily made by so that 2-Hydroxyethyl methacrylate is reacted with commercially available polysiloxanes.
The study found that the stability of plastics in the oral cavity can be improved by introducing Si keys in polymer architecture.In addition, according to
The binding performance of ASTM D 3359-76 test films, Percentage bound have reached 100%；Plastics system is tested according to ASTM D 523
The glossiness of the film obtained, glossiness 75-90.It can be seen that the film can express out the matrix such as tooth excellent associativity, and
And there is gloss and semilustrous characteristic, aesthetic effect can be brought.Further study show that acrylate in copolymer structure
The amount of monomer is more, and the gloss of film is bigger.
In another aspect of this invention, the method prepared according to the aforementioned sodium fluoride anticaries tooth plastics is additionally provided,
This approach includes the following steps：
(1) the sodium fluoride micro mist for taking average grain size to be 2-40 μm is spare, and rosin, frankincense were crushed to 10-100 mesh sieve
It is spare, optional colloidal silicon dioxide, river wax cross 50-300 mesh sieve (i.e. colloidal silicon dioxide, river wax are crossed 50-300 mesh and are sieved, with
Obtain the raw material with required nominal particle size) it is spare.
(2) rosin, frankincense are taken according to each component ratio, 95% ethyl alcohol is added, stirs evenly, stand, 50- complete to dissolving
300 mesh filter；
(3) acrylic resin is added to filtrate, stirs evenly, standing keeps swelling complete, is then optionally added citric acid again
Triethyl stirs evenly；
(4) sodium fluoride and other auxiliary materials are added, ethyl alcohol is added, are uniformly mixed to get sodium fluoride anticaries tooth plastics.
Preferably, wherein the accessory package includes sweetener and/or essential oil.
Preferably, wherein the average grain diameter of the sodium fluoride micro mist is 2-40 μm, preferably 5-20 μm.
Technical scheme of the present invention obtains technique effect following prominent (without being limited thereto)：
(1) it disclosure satisfy that the formulation and technology of solidifying requirements.The fluoride film of the present invention is covered in tooth in the form of emulsion paint
Tooth surface, cures and is able to maintain that after encountering saliva and be present in dental surface, can reach after hardening close with reference product
Performance indicator.Especially when sodium fluoride particle using the present invention and acrylic resin, the performance indicator after curing of coating
It is much better than commercial product, such as 60-80% is improved to the adhesive force of tooth.
(2) the specific fluoride film formula (or prescription) of the present invention disclosure satisfy that release time requires, and fluoride is made to apply
Film can slow release fluoride to avoid fluoride acute poisoning.
(3) present invention uses the reasonable compounding of novel pharmaceutical grade filmogen, that is, rosin, frankincense and acrylic resin, no
It is same as the novel medicinal macromolecule filming material of commercialized product, the filmogen adhesion of the invention is good, water white transparency, system
The sodium fluoride anticaries tooth plastics safety obtained is beautiful.
(4) plastics of the invention, which had in 24 hours, efficiently releases fluorine rate, specifically, the prescription of the present invention has one
Fixed water penetration swellability, it is a kind of hydrophilic back bone type slow-released system to be formed by film, slow and efficient in 24 hours
Fluorine is discharged, ensure that advantage of the product in curative effect.
(5) micromill process of the invention ensure that the stability of suspension.Dissolving of the fluoride in volatile solvent
It spends extremely low, needs the suspension that fluoride is made, the sodium fluoride particle after micronizing is very thin, both can guarantee the stabilization of shield tooth agent
Property, and can guarantee the exquisiteness of sample.
Description of the drawings
Fig. 1 is the SEM figures of the sodium fluoride crystal grain obtained according to embodiment 1；
Fig. 2 is the SEM figures of the sodium fluoride crystal grain obtained according to comparative example 1；
Fig. 3 is the fluorine releasing curve diagram of anti-caries plastics according to the present invention.
Specific implementation mode
Embodiment 1
In batch reactor, it is packed into the half that 1.50mol/L ammonium fluoride solutions reach reactor volume, it then will with pump
0.50mol/L sodium hydroxide solutions are continuously added in reactor, and feeding line is close to reactor wall and it is exported and blender
Impeller tips horizontal aligument, continue feed sodium hydroxide solution until reactor is filled into its final swept volume, hydroxide
Sodium solution feed time is 90 minutes, after addition of the sodium hydroxide solution, takes out gained suspension, is transferred to autoclave
In, hydro-thermal process 10 hours, is not stirred during hydro-thermal at a temperature of 8MPa pressure and 80 DEG C, by reaction system vacuum after hydro-thermal
Middle filtering, is washed with ethanol solution, obtains fluorination sodium crystal.Fig. 1 shows the pattern of fluorination sodium crystal obtained, wherein can be with
It can be clearly seen that sodium fluoride crystal grain has extraordinary pattern.
Comparative example 1
The operation for repeating embodiment 1, differs only in the non-hydrothermal treatment of sodium fluoride.Fig. 2 shows sodium fluoride obtained
The pattern of crystal, surface have the impurity crystal of a small amount of irregular shape.
The sodium fluoride particle that it can be seen from above example and comparative example prepared by the method for the present invention has perfect shape
Looks, to as analyzed above, contribute to the sustained release of fluorine and the mixing with other components in system.
Embodiment 2
The preparation of anti-caries plastics is carried out using the sodium fluoride of embodiment 1, wherein formula is：Sodium fluoride 50g, rosin
10g, frankincense 150g, acrylic resin 200g, 95% ethyl alcohol 1600g；Its preparation process includes：Fluorination prepared by Example 1
Sodium micro mist, and it is spare that rosin, frankincense be crushed to 80 mesh sieve, takes rosin, frankincense according to each component ratio, 95% second is added
Alcohol stirs evenly, and stands, 200 mesh filtration complete to dissolving, and acrylic resin according to the present invention is added to filtrate, stirring is equal
Even, standing keeps swelling complete, stirs evenly, adds sodium fluoride and other auxiliary materials, add ethyl alcohol, is uniformly mixed to get fluorination
Sodium anti-caries plastics.Fig. 3 shows the fluorine releasing curve diagram of the plastics.
By the fluorine release profiles clearly it can be seen from the present invention plastics have especially prolonged slow release effect.
Comparative example 2
Embodiment 2 is repeated, acrylic resin is differed only in and the hundred limited public affairs of Lichuan industry and trade of Beijing (is derived from using commercial product
Department).
Test is found, reaches 40.5% release peak value the fluorine deenergized period of the plastics of comparative example 2 in 12h, then
It begins to decline, it is seen that its fluorine discharges too fast, excessive concentration, and deenergized period is short, hence it is evident that be inferior to according to an embodiment of the invention 2
Product.
Comparative example 3
Comparative example 2 is repeated, differs only in sodium fluoride using sodium fluoride made from comparative example 1.
Test is found, reaches 41.2% release peak value the fluorine deenergized period of the plastics of comparative example 3 in 11.5h, so
After begin to decline, it is seen that the same too fast, excessive concentration of its fluorine release, and deenergized period is short, is also obviously inferior to according to the present invention
Embodiment 2 product.
This written description discloses the present invention, including optimal mode using example, and also enables those skilled in the art
It manufactures and using the present invention.The present invention can patentable scope be defined by the claims, and may include this field skill
Other examples that art personnel expect.If this other examples have not different from the structural elements of the literal language of claims
Element, or if this other examples include with equivalent structure element of the literal language of claims without substantial differences,
Then this other examples are intended within the scope of claims.In the case where inconsistent degree will not be caused, by reference to
It will be incorporated herein in place of all references referred to herein.
Claims (7)
1. a kind of sodium fluoride anticaries tooth plastics, which includes following component in parts by weight：
The average grain diameter of sodium fluoride is 2-40 μm in the plastics, and the sodium fluoride is the crystalline substance with face-centred cubic structure
Grain, the sodium fluoride are made by method comprising the following steps：
(1) in batch reactor, loading ammonium fluoride solution reaches about half of reactor volume, then uses pump by sodium hydroxide
Solution is continuously added in reactor, and sodium hydroxide solution feeding line is close to reactor wall and the impeller of its outlet and blender
Most advanced level is aligned；
(2) continue to feed sodium hydroxide solution until reactor is filled into its final swept volume, sodium hydroxide solution charging reaches
It is known as feed time to the time needed for the final working volume of reactor, feed time was controlled at 60-90 minutes；
(3) after addition of the sodium hydroxide solution, take out gained suspension, be transferred in autoclave, in 5-10MPa pressure and
Hydro-thermal process 6-12 hours at a temperature of 80-120 DEG C, do not stirred during hydro-thermal；
(4) it will filter in reaction system vacuum after hydro-thermal, washed with ethanol solution, obtain fluorination sodium crystal；
Wherein, in step (1), the reactant concentration of ammonium fluoride and sodium hydroxide is 0.30-3.50mol/L independently of one another,
Step (1) carries out at a temperature of 20-50 DEG C；
The acrylic resin is the acrylic resin containing repetitive unit shown in lower formula (I)：
The number-average molecular weight of the acrylic resin is 300-10000.
2. sodium fluoride anticaries tooth plastics according to claim 1, which also includes the river wax of 2-10 parts by weight.
3. sodium fluoride anticaries tooth plastics according to claim 1, which also includes the colloidal state two of 2-10 parts by weight
Silica.
4. sodium fluoride anticaries tooth plastics according to any one of the preceding claims, which also includes 10-45 weights
Measure the triethyl citrate of part.
5. sodium fluoride anticaries tooth plastics according to any one of claim 1-3, which also includes suitable sweet tea
Taste agent and/or essential oil.
6. sodium fluoride anticaries tooth plastics according to any one of claim 1-3, the total weight parts of the plastics are
5000 parts.
7. sodium fluoride anticaries tooth plastics according to claim 1, the average grain diameter of sodium fluoride is 5-20 μ in the plastics
m。
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| CN108524290A (en) * | 2018-06-28 | 2018-09-14 | 吉林省登泰克牙科材料有限公司 | Pre- composite for preventing dental caries of dentistry and preparation method thereof |
| CN115554334A (en) * | 2022-09-23 | 2023-01-03 | 拜斯特药业(广州)有限公司 | Caries preventing coating agent capable of being applied to teeth and having relieving effect and preparation method thereof |
| CN117205116A (en) * | 2023-08-22 | 2023-12-12 | 山东沪鸽口腔材料股份有限公司 | Fluorine anticarious agent with high stability and high fluorine release efficiency and preparation method thereof |
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| US20070041913A1 (en) * | 2003-08-27 | 2007-02-22 | Hanix Co., Ltd. | Tooth coating composition |
| AR071183A1 (en) * | 2008-04-04 | 2010-06-02 | Colgate Palmolive Co | ORAL COMPOSITION THAT INCLUDES AN ACTIVE COMPONENT AND AN ADHESIVE FILM FORMING COMPONENT, METHOD |
| RU2582217C2 (en) * | 2011-09-14 | 2016-04-20 | Колгейт-Палмолив Компани | Teeth whitening strip |
| CN103211710A (en) * | 2013-03-20 | 2013-07-24 | 中国人民解放军第四军医大学口腔医院 | Hydraulic fluoride varnish material |
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| CN107648055A (en) | 2018-02-02 |
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