CN108128797B - A kind of intercalated houghite and preparation method thereof and tooth whitening gel - Google Patents
A kind of intercalated houghite and preparation method thereof and tooth whitening gel Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/042—Gels
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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Abstract
The present invention provides a kind of intercalated houghites and preparation method thereof and tooth whitening gel, belong to daily use chemicals processing technique field, and the element composition of intercalated houghite provided by the invention is shown below: MII 1‑xMIII x(OH)y](An‑)x/n·mH2O, 0.2≤x≤0.8；The MIIIncluding zinc and/or calcium, the MIIIFor aluminium, the An‑For soluble intercalant anion or intercalated molecule, the integer that the n is 0~4；The integer that the y is 1~30, the integer that the m is 1~20.The intercalated houghite is applied to tooth whitening gel, using the photocatalytic activity of zinc-containing hydrotalcite, bleaching power is promoted according to oxidisability electron hole is generated by fill-in light, makes it that can show efficient whitening effect under conditions of harmless.
Description
Technical field
The present invention relates to daily use chemicals processing technique fields more particularly to a kind of intercalated houghite and preparation method thereof and tooth beauty
White gel.
Background technique
The main ingredient that traditional tooth whitening gel is includes that high-strength hydrogen peroxide, the carbomer of urea peroxide are solidifying
Glue.Wherein hydrogen peroxide is its main whitening additive, plays effect by the oxidisability of hydrogen peroxide, realizes dental bleaching
Purpose.But high-strength hydrogen peroxide is corrosive, and can damage to oral mucosa, causes the swollen sense of acid, and be easy to tooth
Structural destruction is caused, health is influenced.
Summary of the invention
In view of this, it is an object of that present invention to provide a kind of intercalated houghites and preparation method thereof and tooth whitening gel.
By intercalated houghite provided by the invention addition in tooth whitening gel, on the basis of improving whitening effect, keep gel whole
PH and human oral cavity pH are maintained in same range, mild non-stimulated, reduce human body harm, realize the tooth beauty of highly effective and safe
It is white.
The present invention provides a kind of intercalated houghite, chemical general formula is as follows:
MII 1-xMIII x(OH)y](An-)x/n·mH2O, 0.2≤x≤0.8；
The MIIIncluding zinc and/or calcium, the MIIIFor aluminium, the An-For soluble intercalant anion or molecule；
The integer that the n is 0~4, the integer that the y is 1~30, the integer that the m is 1~20.
Preferably, the MIIIt further include magnesium.
Preferably, the soluble intercalant anion includes carbonate, nitrate anion, sulfate radical, chloride ion, dodecyl sulphur
Acid group, the solubility intercalated molecule is xylitol.
The present invention also provides the preparation methods of the intercalated houghite, comprising the following steps:
By soluble divalent metal salt, aluminum soluble salt, soluble surfactant, soluble intercalant anion or divide
Son, alkali source are mixed with water carries out coprecipitation reaction, obtains intercalated houghite；The soluble divalent metal salt includes soluble Zn
Salt and/or calcium salt.
Preferably, the soluble zinc salt includes zinc nitrate, zinc chloride or zinc sulfate；The soluble calcium salt includes nitric acid
Calcium, calcium chloride.
Preferably, the aluminum soluble salt includes aluminum nitrate, aluminium chloride or aluminum sulfate.
Preferably, the soluble surfactant include lauryl sodium sulfate, monoglyceride, polyglycerol ester, sucrose ester,
Sapn or tween.
Preferably, the alkali source includes urea, hexamethylenetetramine or sodium hydroxide or potassium hydroxide.
The present invention also provides a kind of tooth whitening gel, the composition including following parts by weight:
Or the intercalated houghite that above-mentioned preparation method obtains.
Preferably, the gelling agent includes card wave 940 or card wave 980, and the desensitizer includes calcirm-fluoride, single fluorophosphoric acid
Sodium, potassium nitrate, strontium fluoride, strontium acetate or oxalates.
Advantageous effects: the element composition of intercalated houghite provided by the invention is shown below: MII 1-xMIII x
(OH)y](An-)x/n·mH2O, 0.2≤x≤0.8；The MIIIncluding zinc and/or calcium, the MIIIFor aluminium, the An-For solubility
Intercalant anion or molecule, the integer that the n is 0~4；The integer that the y is 1~30, the integer that the m is 1~20.
The present invention is using zinc-aluminium or the photocatalytic activity of calcium aluminum hydrotalcite, by fill-in light according to generation oxidisability electron hole
Bleaching power is promoted, makes it that can show efficient whitening effect under conditions of harmless；Calcium aluminum hydrotalcite is to receive
Meter ruler cun, and there is the structure similar with tooth main component hydroxyapatite, facilitate diffusion of active ingredient and is adsorbed in tooth
Tooth surface promotes hydrogen peroxide effective component to work under the irradiation of blue light in the decomposition of dental surface continuous uniform, realizes whitening
The effect of tooth；Again because hydrotalcite shows as alkalescent, the acidity of peroxide can be neutralized, is added in tooth whitening gel,
On the basis of improving whitening effect, it is maintained at gel entirety pH and human oral cavity pH in same range, it is mild non-stimulated, it reduces
Human body harm, realizes the tooth whitening of highly effective and safe；Further, since the hydrotalcite material of preparation is nano-scale, not only more hold
It is easily adsorbed in dental surface to bleach for pigment, and unnecessary material addition can be reduced using itself as dispersible carrier,
Reduce body metabolism toxicity.
Detailed description of the invention
Fig. 1 is to obtain the X-ray powder diffraction figure of zinc-aluminium intercalated houghite Yu common zinc-aluminum hydrotalcite sample in embodiment 1
Spectrum；
Fig. 2 is zinc-aluminium intercalated houghite scanning electron microscope spectrogram in embodiment 1；
Fig. 3 is zinc-aluminium intercalated houghite high-resolution-ration transmission electric-lens spectrogram made from embodiment 1；
Fig. 4 is zinc-aluminium intercalated houghite ultraviolet-visible absorption spectroscopy made from the embodiment of the present invention 1；
Fig. 5 is the gel of the intercalated houghite containing zinc-aluminium in the embodiment of the present invention 5 and common tooth whitening gel to potassium iodide
Oxidability test chart；
Fig. 6 is that the gel of the intercalated houghite containing zinc-aluminium and common tooth whitening gel are yellowish green to calcium in the embodiment of the present invention 6
The bleaching power test chart of plain color element；
Fig. 7 is that the gel of the intercalated houghite containing zinc-aluminium and common tooth whitening gel are red to core block in the embodiment of the present invention 7
The bleaching power test chart of pigment.
Specific embodiment
The present invention provides a kind of intercalated houghite, chemical general formula is as follows:
MII 1-xMIII x(OH)y(An-)x/n·mH2O, 0.2≤x≤0.8；
The MIIIncluding zinc and/or calcium, the MIIIFor aluminium, the An-For soluble intercalant anion or molecule；
The integer that the n is 0~4, the integer that the y is 1~30, the integer that the m is 1~20.
In the present invention, the MIIIncluding zinc and/or calcium, the MIIPreferably one or both of zinc and calcium, it is more excellent
It is selected as zinc.
In the present invention, the MIIFurther include magnesium, works as MIIWhen including magnesium, the MIIThe preferably mixture of zinc and magnesium, calcium
With the mixture of the mixture or zinc of magnesium, magnesium and calcium, the more preferably mixture of zinc and magnesium.
In the present invention, work as MIIFor two kinds and when two or more mixture, the present invention is to each element in intercalated houghite
Proportion be not particularly limited, select proportion well known to those skilled in the art.
In the present invention, the partial size of the intercalated houghite is preferably 50~500nm, more preferably 100~200nm.
The soluble intercalant anion described in the present invention preferably includes carbonate, nitrate anion, sulfate radical, chloride ion, ten
Dialkyl sulfates, it more preferably includes carbonate, nitrate anion or xylitol that the solubility intercalated molecule, which is xylitol,.At this
In invention, the mobile degree of the characteristic diffraction peak of [003] crystal face of the solubility intercalant anion or molecule is preferably 3~10
Degree, more preferably 5~7 degree.
The present invention also provides the preparation methods of the intercalated houghite described in above-mentioned technical proposal, comprising the following steps:
By soluble divalent metal salt, aluminum soluble salt, soluble surfactant, soluble intercalant anion or divide
Son, alkali source are mixed with water carries out coprecipitation reaction, obtains intercalated houghite；The soluble divalent metal salt includes soluble Zn
Salt, soluble calcium salt.
The present invention is by soluble divalent metal salt, aluminum soluble salt, soluble surfactant, soluble intercalant anion
Or molecule, alkali source mix with water and carry out coprecipitation reaction, obtain coprecipitated product.
In the present invention, the temperature of the coprecipitation reaction is preferably 90~130 DEG C, and more preferably 110 DEG C；It is described coprecipitated
The time of shallow lake reaction is preferably 6~48h, more preferably 12~for 24 hours.
In the present invention, the soluble divalent metal salt, aluminum soluble salt, soluble surfactant, solubility are inserted
The molar ratio of layer anion or molecule, alkali source is preferably 2~4:1:0.5~2:1:6~10, more preferably 2:1:1:1:8~9；
The present invention does not have any special restriction to the dosage of the water, can guarantee soluble divalent metal salt, aluminum soluble salt, can
Soluble surfactants, soluble intercalant anion or molecule and alkali source can sufficiently dissolve.
In the present invention, the divalent metal salt includes one or both of soluble zinc salt and soluble calcium salt；Institute
Stating soluble zinc salt is preferably zinc nitrate, zinc chloride or zinc sulfate, more preferably zinc nitrate, zinc chloride；The soluble calcium salt
Preferably zinc nitrate, zinc chloride, more preferably zinc nitrate.
In the present invention, as M in the intercalated houghiteIIWhen further including magnesium, it is also preferable to include can for the divalent metal salt
Soluble magnesium salt, the soluble magnesium salt are preferably magnesium nitrate, magnesium chloride, more preferably magnesium nitrate.
In the present invention, the aluminum soluble salt is preferably aluminum nitrate, aluminium chloride or aluminum sulfate, more preferably aluminum nitrate or
Aluminium chloride.
In the present invention, the soluble surfactant be preferably lauryl sodium sulfate, monoglyceride, polyglycerol ester,
Sucrose ester, sapn or tween, more preferably lauryl sodium sulfate, monoglyceride, sucrose ester or tween, most preferably dodecyl
Sodium sulphate or monoglyceride.In the present invention, when the intercalated molecule Yishui River hard to tolerate, the cosurfactant auxiliary anion is common
Intercalation.
In the present invention, the alkali source is preferably urea, hexamethylenetetramine, sodium hydroxide or potassium hydroxide, more preferably
For urea, hexamethylenetetramine or sodium hydroxide.
The present invention is to the soluble divalent metal salt, aluminum soluble salt, soluble surfactant, soluble intercalation yin
The not special restriction of the sequence that lewis' acid, alkali source are mixed with water, using order by merging well known to those skilled in the art
, in embodiments of the present invention, preferably by the soluble divalent metal salt, aluminum soluble salt, soluble surfactant,
Soluble intercalant anion or molecule and alkali source are added to the water simultaneously；The present invention is not any to the mixed concrete mode
Special restriction in embodiments of the present invention, is preferably stirred using hybrid mode well known to those skilled in the art,
More preferably mechanical stirring, the present invention do not have special restriction to the churned mechanically time, revolving speed, can guarantee mixture
System is uniformly mixed.
After the completion of coprecipitation reaction, obtained coprecipitated product is preferably separated by solid-liquid separation by the present invention, obtains solid production
Object, the solid product are intercalated houghite.The present invention does not have any special restriction to the concrete mode of the separation of solid and liquid,
It preferably filters in the present invention.
After obtaining solid product, solid product is preferably successively washed and is dried by the present invention, obtains intercalated houghite.
In the present invention, the preferred water of the washing and ethyl alcohol alternately wash, and the present invention is to the washing and ethanol washing
Number is preferably 4~8 times, and more preferably 5~6 times；The present invention is not particularly limited the dosage of the cleaning solvent, selects this
Dosage known to the technical staff of field.The present invention does not have special restriction to the concrete mode of the drying, using ability
Known to field technique personnel, the mode of water in solid product can be removed.
The present invention is by soluble divalent metal salt (zinc salt and/or calcium salt), aluminum soluble salt, surfactant, intercalation
Anion or molecule and water obtain intercalated houghite, using zinc-containing hydrotalcite or the photocatalytic activity of calcic hydrotalcite, by auxiliary
It helps illumination to generate oxidisability electron hole and promotes bleaching power, show it can under conditions of harmless efficiently
Whitening effect；Again because hydrotalcite shows as alkalescent, the acidity of peroxide can be neutralized, its harm to human body is reduced；In addition,
Since the hydrotalcite material of preparation is nano-scale, not only it is easier to be adsorbed in dental surface for pigment bleaching, but also can be with
Itself reduces unnecessary material addition, reduces body metabolism toxicity as dispersible carrier.
The present invention also provides a kind of tooth whitening gel, the component including following parts by weight:
The intercalated houghite that preparation method described in stone or above-mentioned technical proposal obtains.
In the present invention, the gelling agent is preferably card wave 940, card wave 980, more preferably card wave 940；The desensitizer
Preferably calcirm-fluoride, sodium monofluorophosphate, potassium nitrate, strontium fluoride, strontium acetate or oxalates, more preferably calcirm-fluoride, single fluorophosphoric acid
Sodium or potassium nitrate.
The present invention does not have special restriction to the preparation method of the tooth whitening gel, ripe using those skilled in the art
The preparation method for the composition known is made.
Intercalated houghite provided by the invention and preparation method thereof and tooth whitening gel are carried out below with reference to embodiment
Detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Zinc nitrate Zn (NO3)2·6H2O, aluminum nitrate Al (NO3)3·9H2O, lauryl sodium sulfate, xylitol and hydroxide
Sodium is added in 800ml deionized water according to the molal quantity of 1.6,0.8,0.4 and 8mmol respectively sufficiently to be dissolved, then by solution
It is placed under 110 DEG C of environment and heats for 24 hours, be then sufficiently dried to obtain zinc-aluminium intercalated houghite with deionized water and ethyl alcohol exchange washing
Zn2Al-LDH.Consisting of Zn2Al(OH)14(C12H25SO4)(C5H12O5)4·9H2O。
X-ray powder diffraction analysis is carried out to zinc-aluminium intercalated houghite in embodiment 1, as a result as shown in Figure 1, wherein A is
Common zinc-aluminum hydrotalcite sample, B are that zinc-aluminium intercalated houghite sample is exchanged by intercalation as seen from Figure 1 in embodiment 1
Reaction, the characteristic diffraction peak for belonging to [003] crystal face of the LDH of intercalant anion or molecule are moved to 7.5 degree from 12.0 degree,
It proves that intercalant anion enters hydrotalcite layers, forms ideal intercalation configuration.
Electron microscope analysis is scanned to product in embodiment 1, as a result as shown in Fig. 2, amplification factor is about 100,000 times, by scheming
2 as can be seen that zinc-aluminium intercalated houghite obtained in embodiment 1 has hexagonal structure, and particle size uniformity is distributed in 200nm
Left and right.
High-resolution-ration transmission electric-lens analysis is carried out to zinc-aluminium intercalated houghite made from embodiment 1, as a result as shown in figure 3, putting
Big multiple is about 500,000 times, from the figure 3, it may be seen that intercalated houghite material has laminated structure, pattern is uniform complete.
To zinc-aluminium intercalated houghite made from embodiment 1 carry out ultraviolet-visible absorption spectroscopy analysis, as a result as shown in figure 4,
As seen from Figure 4, there is apparent absorption in 450 nano wave lengths, since it has the characteristic of semiconductor of similar zinc oxide, inhales
The photon of receipts can be converted into electron hole pair, and sufficiently demonstrating it and can use blue light and generate, there is the hole of oxidisability to realize
Whitening effect.
Embodiment 2
Calcium nitrate Ca (NO3)2·6H2O, aluminum nitrate Al (NO3)3·9H2O, lauryl sodium sulfate, xylitol and urea point
It is not added in 1000ml deionized water according to the amount of 4mmol, 1mmol, 1mmol and 10mmol and sufficiently dissolves, then by solution
It is placed under 90 DEG C of environment and heats 72h progress coprecipitation reaction, produced after separation of solid and liquid with deionized water and ethyl alcohol exchange washing solid
Object is sufficiently dried to obtain calcium aluminium intercalated houghite.Consisting of Ca2Al(OH)14(C12H25SO4)2(C5H12O5)6·9H2O。
Embodiment 3
Zinc nitrate Zn (NO3)2·6H2O, calcium nitrate Ca (NO3)2·6H2O, aluminum nitrate Al (NO3)3·9H2O, dodecyl
Sodium sulphate, xylitol and sodium hydroxide are added to 1000ml according to the amount of 1mmol, 1mmol, 1mmol, 0.5 and 10mmol respectively
It is sufficiently dissolved in deionized water, molal quantity is respectively 1,1,1,0.5 and 10mmol, and then solution is placed under 110 DEG C of environment
Heating for 24 hours, is then sufficiently dried to obtain zinc-aluminium intercalated houghite ZnCaAl-LDH with deionized water and ethyl alcohol exchange washing.Its group
As ZnCaAl (OH)12(C12H25SO4)(C5H12O5)4·9H2O。
Embodiment 4
5.0g card wave 940 is dissolved in 500mL water, is sufficiently swollen, 4h or so, until being formed and being stablized without solid without white powder
Gel.Continuously stir be added dropwise triethanolamine 5.0g to colloidal sol be it is colorless and transparent thick, pH is about 5.5 ± 0.5.Nanometer two
Silica 0.1g, zinc-aluminum hydrotalcite additive 1.0g, xylitol 1.0g and calcirm-fluoride 1g are evenly dispersed to appropriate in embodiment 1
25% hydrogen peroxide 120mL is added in deionized water, after fully dispersed, before being added in the 500ml card wave gel-type vehicle of swelling,
It stirs evenly, obtains the tooth whitening gel of the intercalated houghite containing zinc-aluminium.
Comparative example 1
Zinc-aluminum hydrotalcite additive in embodiment 4 is replaced with into common additives titanium dioxide in the prior art,
Its condition is same as Example 4, obtains common tooth whitening gel.
Embodiment 5
The tooth of the common tooth whitening gel in comparative example 1 and the intercalated houghite containing zinc-aluminium in embodiment 1 is taken respectively
After each 1mL of tooth whitening gelatin dilutes ten times, 1mL is added dropwise respectively into pre-configured liquor kalii iodide, under the same conditions
(about 420 nano wave length blue light) carries out illumination, then tests within the set time solution absorbance, by absorbing peak intensity
The concentration to judge the iodine of iodide ion oxidation generation in solution is spent, further reflects the oxidability of gel.As shown in figure 5,
Under identical initial concentration and external condition, the gel that joined hydrotalcite component can be such that potassium iodide aoxidizes faster, oxygen
Change capability improving about 44%.
Embodiment 6
Liquor kalii iodide in embodiment 5 is replaced with into calcein solution, other conditions are same as Example 5.It is tied
For fruit as shown in fig. 6, under identical initial concentration and external condition, the whitening gelatin that joined intercalated houghite component can be faster
So that pigment oxidation is decolourized, calcein pigment bleaching effect promoted about 35%.
Embodiment 7
Liquor kalii iodide in embodiment 5 is replaced with into the red Solutions Solution of core block, other conditions are same as Example 5.Its
As a result as shown in fig. 7, under identical initial concentration and external condition, the gel that joined zinc-aluminum hydrotalcite component can be faster
Pigment oxidation is set to decolourize, the red Solutions Solution bleaching effect of core block promotes about 35%.
The present invention is the above is only a preferred embodiment of the present invention, it is noted that for the common of the art
For technical staff, various improvements and modifications may be made without departing from the principle of the present invention, these are improved and profit
Decorations also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of tooth whitening gel, the component including following parts by weight:
The intercalated houghite has chemical general formula shown in Formulas I:
MII 1-xMIII x(OH)y(An-)x/n·mH2O Formulas I, 0.2≤x≤0.8；The MIIIncluding zinc and/or calcium, the MIIIFor aluminium,
The An-For soluble intercalant anion or molecule；
The integer that the n is 0~4, the integer that the y is 1~30, the integer that the m is 1~20.
2. tooth whitening gel according to claim 1, which is characterized in that the MIIIt further include magnesium.
3. tooth whitening gel according to claim 1, which is characterized in that the solubility intercalant anion includes carbonic acid
Root, nitrate anion, sulfate radical, chloride ion, dodecyl sulphate root, the solubility intercalated molecule is xylitol.
4. tooth whitening gel according to any one of claims 1 to 3, which is characterized in that the intercalated houghite
Preparation method, comprising the following steps:
By soluble divalent metal salt, aluminum soluble salt, soluble surfactant, soluble intercalant anion or molecule, alkali
Source is mixed with water carries out coprecipitation reaction, obtains intercalated houghite；The soluble divalent metal salt include soluble zinc salt and/
Or soluble calcium salt；
M in the intercalated houghite shown in the Formulas IIIWhen further including magnesium, the soluble divalent metal salt further includes soluble magnesium
Salt.
5. tooth whitening gel according to claim 4, which is characterized in that the soluble zinc salt includes zinc nitrate, chlorine
Change zinc or zinc sulfate；The soluble calcium salt includes calcium nitrate and calcium chloride.
6. tooth whitening gel according to claim 4, which is characterized in that the aluminum soluble salt includes aluminum nitrate, chlorine
Change aluminium or aluminum sulfate.
7. tooth whitening gel according to claim 4, which is characterized in that the soluble surfactant includes 12
Sodium alkyl sulfate, monoglyceride, polyglycerol ester, sucrose ester, sapn or tween.
8. tooth whitening gel according to claim 4, which is characterized in that the alkali source includes urea, six methines four
Amine, sodium hydroxide or potassium hydroxide.
9. tooth whitening gel according to claim 1, which is characterized in that the gelling agent is card wave, the desensitizer
Including calcirm-fluoride, sodium monofluorophosphate, potassium nitrate, strontium fluoride, strontium acetate or oxalates.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711477394.XA CN108128797B (en) | 2017-12-29 | 2017-12-29 | A kind of intercalated houghite and preparation method thereof and tooth whitening gel |
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| CN201711477394.XA CN108128797B (en) | 2017-12-29 | 2017-12-29 | A kind of intercalated houghite and preparation method thereof and tooth whitening gel |
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