CN108190899A - A kind of preparation method of the colored silicon dioxide granule of toothpaste - Google Patents
A kind of preparation method of the colored silicon dioxide granule of toothpaste Download PDFInfo
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- CN108190899A CN108190899A CN201810167179.8A CN201810167179A CN108190899A CN 108190899 A CN108190899 A CN 108190899A CN 201810167179 A CN201810167179 A CN 201810167179A CN 108190899 A CN108190899 A CN 108190899A
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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
- A61K8/046—Aerosols; Foams
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/86—Polyethers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/48—Thickener, Thickening system
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Abstract
The invention discloses a kind of toothpaste preparation methods of colored silicon dioxide granule, it is characterised in that:Add 18m into reactor one3Sodium sulphate, then add the ethoxylated dodecyl alcohol of 6kg;Sodium silicate solution is added in into reactor one again, sulfuric acid solution is added after 2min, until reaction end pH value is 3;Carboxymethylcellulose sodium solution is added in into reactor two, then adds sulfuric acid solution, solution ph is adjusted to 6.5, adds potassium peroxydisulfate and sodium hydrogensulfite, the sodium carboxymethylcellulose of activation is made;It is finally 10 by weight by the sodium carboxymethylcellulose of activation and food grade colorant solution:1 ratio is added in reactor one, press filtration, is beaten filter cake 3 hours under 3000r/min, and re-dry crushes, and obtains colored silicon dioxide granule.Colored silicon dioxide granule prepared by the present invention can reduce the defoaming to toothpaste foaming agent, improve foaming abundancy degree and scrub mouthfeel.
Description
Technical field
The present invention relates to chemical industry field of inorganic material preparing technology more particularly to a kind of colored silicon dioxide granules of toothpaste
Preparation method.
Background technology
Toothpaste has friction effect and removal bacterial plaque, and cleaning polishing facing makes the effect of oral cavity refreshing.At present on the market
Toothpaste is divided into ordinary toothpaste, fluoride dental cream and medicated toothpaste three categories.The main ingredient of ordinary toothpaste includes abrasive, cleaning
Agent, wetting agent, preservative, foaming agent and aromatic have the function of that general toothpaste shares.With development in science and technology, it has been found that
Fluoride can be with the effect of preventing decayed tooth, and for many years it was verified that fluoride is with after teeth contact, making easily sour in dental tissue
The apatite hydroxide of dissolving forms less soluble fluor-apatite, so as to improve the resistance to corrosion of tooth.Medicated toothpaste is then
Add certain drug on the basis of ordinary toothpaste, toothpaste is reached in dental surface or tooth ambient enviroment when brushing teeth, and passes through drug
Effect, reduce plaque, so as to play the role of anti-dental caries and periodontosis.
At present, medicated toothpaste pole is favored by people, and has effects that prevention or therapeutic efficiency using toothpaste to promote
Drug be a kind of comparatively ideal mode.But medicated toothpaste also has its unfavorable aspect, first, toothpaste cannot be kept too in mouth
For a long time, that is, it is gargled, drug is made to be difficult to play drug effect in a short time, and special medicament dosage must also avoid stimulation mouth
Interior soft tissue, thus enough effective concentrations cannot be increased to, the effect of toothpaste in itself is often hindered or by dirt in mouth by form
Feature limits, thus is difficult to reach the region really fallen ill.Secondly, often due to standing time is long it occurs for the drug in toothpaste
Its chemical change loses original drug effect, and Chang Yin is unsuitable for being put into toothpaste active drug with peculiar smell again, in addition with medicine
The problem of object drug resistance.
Either what kind of toothpaste, abrasive and foaming agent are all the important components of formulation of tooth-paste, titanium dioxide
Silicon has good friction cleaning capacity, therefore be widely used in toothpaste and match because molecular structure is unique, physicochemical properties are stablized
Fang Zhong.But silica due to grain size is small, large specific surface area, surface can be high, there is tridimensional network, thus absorption property compared with
By force, stronger suction-operated can be generated to bubble, so as to which the foam generated to toothpaste foaming agent has certain defoaming to act on, reduced
Foaming abundancy degree when brushing teeth, affect toothpaste scrub mouthfeel.
Publication No. CN 102993782A, publication date are that the Chinese patent literature of on 03 27th, 2013 discloses one kind
The preparation method of polyurethane acrylates oligomer surface modified silicon dioxide, it is characterised in that follow the steps below:
(1)Sol-gel method synthesizes nano silicon dioxide and its modification:It is 53.6 by volume:3.1:1:2 weigh absolute ethyl alcohol, dense
The ammonium hydroxide for 28%, deionized water, tetraethyl orthosilicate are spent, said components are uniformly mixed, it is small that 50 DEG C of constant temperature is stirred to react 24
When, obtain silica ethanol solution;Silane coupling agent, silane coupling agent are added in into above-mentioned silica ethanol solution:Just
The volume ratio of tetraethyl orthosilicate is 0.1:1-1:1;50 DEG C of constant temperature is stirred to react 24 hours, with after ethyl alcohol centrifuge washing 3 times i.e.
Obtain silane-modified silica;(2)The synthesis of isocyanate-terminated polyurethane acrylates oligomer:By two isocyanides
Esters of gallic acid monomer is 1.1 with acrylic ester monomer molar ratio:1 proportioning, by acrylic ester monomer be slowly dropped to added with
In the isocyanate monomers of catalyst, 50 DEG C of constant temperature is stirred to react 2-2.5 hours, obtains isocyanate-terminated polyurethane
Acrylate quasi-oligomer;The catalyst selects dibutyltin dilaurate or stannous octoate;Its dosage is diisocyanate
The 0.05%-0.5% of esters monomer and acrylic ester monomer quality sum;(3)Polyurethane acrylates oligomer surface changes
The synthesis of property silica:By above-mentioned steps(1)In silane-modified silica ultrasonic disperse in dehydration acetone, by silane
Modified silica:The mass ratio of isocyanate-terminated polyurethane acrylates oligomer is 1:1-1:10 proportioning
Step is added in thereto(2)The isocyanate-terminated polyurethane acrylates oligomer of gained, normal-temperature reaction 3 hours,
Polyurethane acrylates oligomer surface modified silicon dioxide is obtained after centrifuge washing.
The preparation method of polyurethane acrylates oligomer surface modified silicon dioxide disclosed in the patent document, system
Standby obtained silica, although having dispersibility and stability well in the organic solvents such as toluene, ethyl acetate,
There is no the defoaming sex chromosome mosaicisms for solving silica, are prepared for toothpaste, foaming abundancy degree or relatively low, shadow are produced when brushing teeth
Sound scrubs mouthfeel.
Invention content
The defects of present invention is in order to overcome the above-mentioned prior art provides a kind of preparation of the colored silicon dioxide granule of toothpaste
Method, colored silicon dioxide granule prepared by the present invention can effectively reduce the defoaming to toothpaste foaming agent, and it is rich to improve foam
Rich degree and scrub mouthfeel.
The present invention is achieved through the following technical solutions:
A kind of preparation method of the colored silicon dioxide granule of toothpaste, it is characterised in that:18m is added in into reactor one3Sulfuric acid
Sodium solution adds the ethoxylated dodecyl alcohol of 6kg, stirs evenly and is heated to 75 DEG C;Again silicon is added in into reactor one
Acid sodium solution adds sulfuric acid solution after 2min, until reaction end pH value is 3, stops addition sulfuric acid solution;Toward reactor two
Middle addition carboxymethylcellulose sodium solution stirs 8min at 75 DEG C, then adds sulfuric acid solution, and solution ph is adjusted to 6.5, then add
Enter potassium peroxydisulfate and sodium hydrogensulfite, and stir evenly, the sodium carboxymethylcellulose of activation is made;Finally by the carboxymethyl of activation
Sodium cellulosate and food grade colorant solution are 10 by weight:1 ratio is added in reactor one, after reacting 8h at 50 DEG C
Filter cake is beaten 3 hours by press filtration with high speed dispersor under 3000r/min, and re-dry crushes, and obtains colored titanium dioxide silicon grain
Son.
The potassium peroxydisulfate and the weight ratio of sodium hydrogensulfite of adding in is 3:1, speed of agitator 3500r/min.
The mass percent concentration of carboxymethylcellulose sodium solution is 8-10% in the reactor two, and sulfuric acid solution rubs
You are a concentration of 8-10mol/L.
The Average Particle Diameters of the colour silicon dioxide granule are 26 μm.
The food grade colorant solution is the sorbierite or polyglycol solution of food-grade.
The beneficial effects of the invention are as follows:
It is 10 by weight by the sodium carboxymethylcellulose of activation and food grade colorant solution:1 ratio is added to reactor one
In, after reacting 8h at 50 DEG C, solids is obtained by filtration, by solids drying and crushing, obtains colored silicon dioxide granule, grain
Son greatly reduces the RDA value of particle in spherical porous structure, the porous structure of the spherical shape, and clean-up performance is preferable, Er Qieqiu
The particle of shape has clearly demarcated sharp corner angle unlike other dentifrice abrasives, therefore will not damage enamel, several to tooth
It will not cause any damage.As abrasive, not only with good friction clean-up performance, but also abrasiveness can be reduced,
In addition, also having good foaming agent compatibility, toothpaste is made to have good clean-up performance and abundant foam when scrubbing, is carried
Height scrubs mouthfeel;Due to colored silicon dioxide granule obtained, kernel is inorganic constituents, and shell is organic principle, thus
Rubbing action and water suction thickening power can be had both in toothpaste simultaneously, be keyed between interior nuclear composition and shell by chemistry, because
This advantage stablized with structure and performance.
Specific embodiment
Embodiment 1
A kind of toothpaste preparation method of colored silicon dioxide granule, 18m is added in into reactor one3Metabisulfite solution, then
The ethoxylated dodecyl alcohol of 6kg is added in, stir evenly and is heated to 75 DEG C;Sodium silicate solution is added in into reactor one again,
Sulfuric acid solution is added after 2min, until reaction end pH value is 3, stops addition sulfuric acid solution;Carboxylic is added in into reactor two
Methylcellulose sodium solution stirs 8min at 75 DEG C, then adds sulfuric acid solution, and solution ph is adjusted to 6.5, adds persulfuric acid
Potassium and sodium hydrogensulfite, and stir evenly, the sodium carboxymethylcellulose of activation is made;Finally by the sodium carboxymethylcellulose of activation
It is 10 by weight with food grade colorant solution:1 ratio is added in reactor one, and press filtration after 8h is reacted at 50 DEG C, is used
Filter cake is beaten 3 hours by high speed dispersor under 3000r/min, and re-dry crushes, and obtains colored silicon dioxide granule.
Embodiment 2
A kind of toothpaste preparation method of colored silicon dioxide granule, 18m is added in into reactor one3Metabisulfite solution, then
The ethoxylated dodecyl alcohol of 6kg is added in, stir evenly and is heated to 75 DEG C;Sodium silicate solution is added in into reactor one again,
Sulfuric acid solution is added after 2min, until reaction end pH value is 3, stops addition sulfuric acid solution;Carboxylic is added in into reactor two
Methylcellulose sodium solution stirs 8min at 75 DEG C, then adds sulfuric acid solution, and solution ph is adjusted to 6.5, adds persulfuric acid
Potassium and sodium hydrogensulfite, and stir evenly, the sodium carboxymethylcellulose of activation is made;Finally by the sodium carboxymethylcellulose of activation
It is 10 by weight with food grade colorant solution:1 ratio is added in reactor one, and press filtration after 8h is reacted at 50 DEG C, is used
Filter cake is beaten 3 hours by high speed dispersor under 3000r/min, and re-dry crushes, and obtains colored silicon dioxide granule.
The potassium peroxydisulfate and the weight ratio of sodium hydrogensulfite of adding in is 3:1, speed of agitator 3500r/min.
The mass percent concentration of carboxymethylcellulose sodium solution is 8% in the reactor two, sulfuric acid solution it is mole dense
It spends for 8mol/L.
The Average Particle Diameters of the colour silicon dioxide granule are 26 μm.
The food grade colorant solution is the sorbierite of food-grade.
Embodiment 3
A kind of toothpaste preparation method of colored silicon dioxide granule, 18m is added in into reactor one3Metabisulfite solution, then
The ethoxylated dodecyl alcohol of 6kg is added in, stir evenly and is heated to 75 DEG C;Sodium silicate solution is added in into reactor one again,
Sulfuric acid solution is added after 2min, until reaction end pH value is 3, stops addition sulfuric acid solution;Carboxylic is added in into reactor two
Methylcellulose sodium solution stirs 8min at 75 DEG C, then adds sulfuric acid solution, and solution ph is adjusted to 6.5, adds persulfuric acid
Potassium and sodium hydrogensulfite, and stir evenly, the sodium carboxymethylcellulose of activation is made;Finally by the sodium carboxymethylcellulose of activation
It is 10 by weight with food grade colorant solution:1 ratio is added in reactor one, and press filtration after 8h is reacted at 50 DEG C, is used
Filter cake is beaten 3 hours by high speed dispersor under 3000r/min, and re-dry crushes, and obtains colored silicon dioxide granule.
The potassium peroxydisulfate and the weight ratio of sodium hydrogensulfite of adding in is 3:1, speed of agitator 3500r/min.
The mass percent concentration of carboxymethylcellulose sodium solution is 9% in the reactor two, sulfuric acid solution it is mole dense
It spends for 9mol/L.
The Average Particle Diameters of the colour silicon dioxide granule are 26 μm.
The food grade colorant solution is the sorbierite of food-grade.
Embodiment 4
A kind of toothpaste preparation method of colored silicon dioxide granule, 18m is added in into reactor one3Metabisulfite solution, then
The ethoxylated dodecyl alcohol of 6kg is added in, stir evenly and is heated to 75 DEG C;Sodium silicate solution is added in into reactor one again,
Sulfuric acid solution is added after 2min, until reaction end pH value is 3, stops addition sulfuric acid solution;Carboxylic is added in into reactor two
Methylcellulose sodium solution stirs 8min at 75 DEG C, then adds sulfuric acid solution, and solution ph is adjusted to 6.5, adds persulfuric acid
Potassium and sodium hydrogensulfite, and stir evenly, the sodium carboxymethylcellulose of activation is made;Finally by the sodium carboxymethylcellulose of activation
It is 10 by weight with food grade colorant solution:1 ratio is added in reactor one, and press filtration after 8h is reacted at 50 DEG C, is used
Filter cake is beaten 3 hours by high speed dispersor under 3000r/min, and re-dry crushes, and obtains colored silicon dioxide granule.
The potassium peroxydisulfate and the weight ratio of sodium hydrogensulfite of adding in is 3:1, speed of agitator 3500r/min.
The mass percent concentration of carboxymethylcellulose sodium solution is 10% in the reactor two, mole of sulfuric acid solution
A concentration of 10mol/L.
The Average Particle Diameters of the colour silicon dioxide granule are 26 μm.
The food grade colorant solution is the polyglycol solution of food-grade.
It is 10 by weight by the sodium carboxymethylcellulose of activation and food grade colorant solution:1 ratio is added to reaction
In device one, after reacting 8h at 50 DEG C, solids is obtained by filtration, by solids drying and crushing, obtains colored titanium dioxide silicon grain
Son, particle are in spherical porous structure, and the porous structure of the spherical shape greatly reduces the RDA value of particle, and clean-up performance is preferable, and
And spherical particle has clearly demarcated sharp corner angle unlike other dentifrice abrasives, therefore will not damage enamel, to tooth
Tooth hardly causes any damage.As abrasive, not only with good friction clean-up performance, but also abrasion can be reduced
Property, in addition, also having good foaming agent compatibility, toothpaste is made to have good clean-up performance and abundant bubble when scrubbing
Mouthfeel is scrubbed in foam, raising;Due to colored silicon dioxide granule obtained, kernel is inorganic constituents, and shell is organic principle, because
And rubbing action and water suction thickening power can be had both simultaneously in toothpaste, connected between interior nuclear composition and shell by chemical bond
It connects, therefore the advantage stablized with structure and performance.
Claims (5)
1. a kind of toothpaste preparation method of colored silicon dioxide granule, it is characterised in that:18m is added in into reactor one3Sulfuric acid
Sodium solution adds the ethoxylated dodecyl alcohol of 6kg, stirs evenly and is heated to 75 DEG C;Again silicon is added in into reactor one
Acid sodium solution adds sulfuric acid solution after 2min, until reaction end pH value is 3, stops addition sulfuric acid solution;Toward reactor two
Middle addition carboxymethylcellulose sodium solution stirs 8min at 75 DEG C, then adds sulfuric acid solution, and solution ph is adjusted to 6.5, then add
Enter potassium peroxydisulfate and sodium hydrogensulfite, and stir evenly, the sodium carboxymethylcellulose of activation is made;Finally by the carboxymethyl of activation
Sodium cellulosate and food grade colorant solution are 10 by weight:1 ratio is added in reactor one, after reacting 8h at 50 DEG C
Filter cake is beaten 3 hours by press filtration with high speed dispersor under 3000r/min, and re-dry crushes, and obtains colored titanium dioxide silicon grain
Son.
2. a kind of toothpaste according to claim 1 preparation method of colored silicon dioxide granule, it is characterised in that:It is described
The weight ratio for adding in potassium peroxydisulfate and sodium hydrogensulfite is 3:1, speed of agitator 3500r/min.
3. a kind of toothpaste according to claim 1 preparation method of colored silicon dioxide granule, it is characterised in that:It is described
The mass percent concentration of carboxymethylcellulose sodium solution is 8-10% in reactor two, and the molar concentration of sulfuric acid solution is 8-
10mol/L。
4. a kind of toothpaste according to claim 1 preparation method of colored silicon dioxide granule, it is characterised in that:It is described
The Average Particle Diameters of colored silicon dioxide granule are 26 μm.
5. a kind of toothpaste according to claim 1 preparation method of colored silicon dioxide granule, it is characterised in that:It is described
Food grade colorant solution is the sorbierite or polyglycol solution of food-grade.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109704349A (en) * | 2019-02-22 | 2019-05-03 | 广州市飞雪材料科技有限公司 | A kind of low-density colour silicon dioxide granule and its preparation with porous structure |
CN117323241A (en) * | 2023-10-24 | 2024-01-02 | 金三江(肇庆)硅材料股份有限公司 | Silica particles for oral cavity as well as preparation method and application thereof |
-
2018
- 2018-02-28 CN CN201810167179.8A patent/CN108190899A/en not_active Withdrawn
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109704349A (en) * | 2019-02-22 | 2019-05-03 | 广州市飞雪材料科技有限公司 | A kind of low-density colour silicon dioxide granule and its preparation with porous structure |
WO2020168662A1 (en) * | 2019-02-22 | 2020-08-27 | 广州市飞雪材料科技有限公司 | Low-density colored silica particles having porous structure, and preparation thereof |
CN117323241A (en) * | 2023-10-24 | 2024-01-02 | 金三江(肇庆)硅材料股份有限公司 | Silica particles for oral cavity as well as preparation method and application thereof |
CN117323241B (en) * | 2023-10-24 | 2024-05-28 | 金三江(肇庆)硅材料股份有限公司 | Silica particles for oral cavity as well as preparation method and application thereof |
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