CN113350205B - High-loading high-cleaning friction type silicon dioxide for dentifrice and preparation method thereof - Google Patents
High-loading high-cleaning friction type silicon dioxide for dentifrice and preparation method thereof Download PDFInfo
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- CN113350205B CN113350205B CN202110686846.5A CN202110686846A CN113350205B CN 113350205 B CN113350205 B CN 113350205B CN 202110686846 A CN202110686846 A CN 202110686846A CN 113350205 B CN113350205 B CN 113350205B
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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
- A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
- A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
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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
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention belongs to the technical field of silicon dioxide, and particularly relates to high-loading-capacity high-cleaning-friction type silicon dioxide for dentifrice and a preparation method thereof. The invention adopts water glass with a certain concentration and a modulus of 1.5-3.5 to react with sulfuric acid with a certain concentration under the action of sodium dodecyl sulfate to prepare the high-load high-cleaning friction type silicon dioxide for the dentifrice. The silicon dioxide for the high-loading high-cleaning friction type dentifrice provided by the invention is high-abrasion high-adsorption precipitated silicon dioxide, has larger particle size, is not easy to disperse, has water absorption of 180mL/100g, can prevent moisture when being applied to the dentifrice, and prevents the dentifrice from absorbing moisture and agglomerating in the dentifrice storage process. In addition, the high-loading high-cleaning friction type silicon dioxide for the dentifrice provided by the invention has high loading capacity and can improve the performance of the dentifrice.
Description
Technical Field
The invention belongs to the technical field of silicon dioxide, and particularly relates to high-loading-capacity high-cleaning-friction type silicon dioxide for dentifrice and a preparation method thereof.
Background
Precipitated silica is widely used as an abrasive and a thickener in toothpaste formulations due to its stable physical properties, high temperature resistance, acid and alkali resistance, environmental friendliness, good cleaning performance and excellent fluorine compatibility. In recent years, the dentifrice gradually exposes the horns in the market and is more widely applied. Dentifrice is widely popular because of its rich taste, good efficacy and portability.
Calcium carbonate or magnesium carbonate is generally adopted as an abrasive agent in the existing dentifrice on the market, the pH value of the dentifrice is generally alkaline, but the oral mucosa can be damaged when the dentifrice is used for brushing teeth under an alkaline condition, so that precipitated silica can be used for replacing calcium carbonate or magnesium carbonate in the dentifrice to be used as an abrasive agent, and meanwhile, the high adsorption performance of the precipitated silica can be used for bearing beneficial components in the dentifrice, such as probiotics, vitamins and the like. However, the existing research on adopting silicon dioxide as a dentifrice abrasive is less, and the existing silicon dioxide has smaller particle size and is applied to dentifrice with too good dispersibility, so that the abrasion type of the dentifrice is reduced. In addition, the existing silicon dioxide has poor water absorption, cannot prevent moisture when being applied to the dentifrice, and is easy to cause the caking phenomenon of the dentifrice. Therefore, in order to improve the properties of high cleaning and easy storage of the dentifrice and improve the living standard of people, the preparation of the high-cleaning high-water-absorption high-adsorption precipitated silica for the dentifrice is necessary.
Patent publication No. CN111544320A discloses an oral composition indicating proper tooth cleaning, comprising at least 0.5% by weight of silica agglomerates, the silica particles of which have an average particle size of 1-50 μm, and the composition has a viscosity of 10-90 BKU. Such oral compositions encourage adequate and complete tooth cleaning, but they contain silica with a smaller average particle size and the compositions have poor dispersibility and thus poor abrasivity.
Patent publication No. CN110623848A discloses a dentifrice for repairing oral mucosa and its preparation method, wherein the formulation comprises abrasive, taste modifier, edible essence, foaming agent, active ingredient and water, wherein the abrasive is at least one of thickening silica and abrasive silica, calcium carbonate, calcium phosphate dihydrate and microcrystalline cellulose. The dentifrice is added with active ingredients containing bioactive glass, has cell repairing function, but the water absorption of silicon dioxide in the abrasive is small, the moisture resistance is poor when the dentifrice is applied to the dentifrice, and the dentifrice is easy to agglomerate.
In conclusion, the technical problems of poor friction type of silicon dioxide, poor water absorption, moisture resistance of the dentifrice, easy caking and the like generally exist in the prior art.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide silicon dioxide for high-loading high-cleaning friction type dentifrice and a preparation method thereof. The silicon dioxide for the high-loading high-cleaning friction type dentifrice provided by the invention is high-abrasion high-adsorption precipitated silicon dioxide, has larger particle size, is not easy to disperse, has water absorption of 180mL/100g, can prevent moisture when being applied to the dentifrice, and prevents the dentifrice from absorbing moisture and agglomerating in the dentifrice storage process. In addition, the high-loading high-cleaning friction type silicon dioxide for the dentifrice provided by the invention has high loading capacity and can improve the performance of the dentifrice.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of silicon dioxide for high-loading capacity high-cleaning friction type dentifrice comprises the following steps:
s1, liquefying solid sodium silicate at high temperature, and adding water to prepare a sodium silicate solution with the concentration of 1.5-3.0 mol/L;
s2, preparing a sulfuric acid solution with the concentration of 4.0-8.0 mol/L;
s3, adding the sodium dodecyl sulfate solution into the reaction kettle, heating to 70-85 ℃, opening a stirring paddle in the reaction kettle, and dropwise adding the sodium silicate solution prepared in the step S1 and the sulfuric acid solution prepared in the step S2 under the stirring state, wherein the dropwise adding amount of the sodium silicate solution is 11.5-13.5m3After the sodium silicate solution is dripped, controlling the reaction temperature to be 80-95 ℃, continuously dripping the sulfuric acid solution until the pH value in the reaction system is 3.5-5.5, continuously stirring, standing and press-filtering to obtain a filter cake;
s4, washing the filter cake obtained in the step S3, and spray-drying the obtained slurry to obtain the filter cake.
Further, the modulus of the solid sodium silicate in the step S1 of the preparation method of the silica for high loading high cleaning friction type dentifrice is 1.5 to 3.5.
Further, the preparation method of the silicon dioxide for the high-loading high-cleaning friction type dentifrice comprises the step S3 of adding 0.10-0.95% of sodium dodecyl sulfate solution by mass and 20-40% of sodium silicate solution by volume.
Further, the stirring frequency of the stirring blade in the step S3 of the preparation method of the silicon dioxide for the high-loading high-cleaning friction type dentifrice is 30-40 Hz.
Further, the dropping speed of the sodium silicate solution in the step S3 of the preparation method of the silicon dioxide for the high-loading high-cleaning friction type dentifrice is 3.5 to 5.0m3H; the dropping speed of the sulfuric acid solution is 2.0-3.0m3/h。
Further, the preparation method of the silicon dioxide for the high-loading high-cleaning friction type dentifrice in the step S3 has the standing time of 20-60 min.
Further, the preparation method of the silica for high loading force high cleaning friction type dentifrice, wherein the particle size of the silica is controlled to be 45 to 60 μm during the spray drying process in step S4.
The invention also provides the silicon dioxide for the high-loading high-cleaning friction type dentifrice, which is prepared by the preparation method of the silicon dioxide for the high-loading high-cleaning friction type dentifrice.
The invention adopts water glass with a certain concentration and a modulus of 1.5-3.5 to react with sulfuric acid with a certain concentration under the action of sodium dodecyl sulfate to prepare the high-load high-cleaning friction type silicon dioxide for the dentifrice. The preparation process of the high-loading high-cleaning friction type silicon dioxide for the dentifrice is simple, the produced silicon dioxide is not required to be subjected to subsequent crushing treatment, the state of larger particle size relative to the silicon dioxide for the toothpaste is kept, the friction effect is increased by mutual collision, and the reduction of the specific surface area is avoided to a certain extent.
In addition, the degree of ionization of anionic surfactants is affected by the ph of the environment, resulting in a resultant system charge density, which determines the curvature of the organic and inorganic surfaces. And in the process that the pH value is gradually changed to be stable, the sodium dodecyl sulfate builds a basic framework for the amorphous silicon dioxide from a cage shape to a cylinder, so that the aggregation and the formation of primary particles are facilitated, and macropores are gradually surrounded to form the characteristic of high adsorbability of the silicon dioxide. At the same time, this characteristic provides a basis for silica as a carrier for macromolecules in dentifrices. In the acid-base reaction process, the reaction in the system can rise, the original reaction temperature of 70-85 ℃ is gradually raised to 80-95 ℃, and friction type silicon dioxide with a compact structure can be generated under the high temperature condition.
Compared with the prior art, the silicon dioxide for the high-loading high-cleaning friction type dentifrice and the preparation method thereof have the following advantages:
(1) the D50 particle size of the high-loading high-cleaning friction type silicon dioxide for the dentifrice is 45-60 mu m, the friction performance is good, and the high-cleaning performance is achieved;
(2) the water absorption capacity of the silicon dioxide for the high-loading high-cleaning friction type dentifrice is 180mL/100g, and the silicon dioxide can prevent moisture when being applied to the dentifrice and prevent the dentifrice from absorbing moisture and agglomerating in the storage process of the dentifrice;
(3) the silicon dioxide for the high-loading high-cleaning friction type dentifrice provided by the invention has high loading capacity and can improve the performance of the dentifrice;
(4) the high-loading high-cleaning friction type silicon dioxide for the dentifrice provided by the invention has a simple preparation process, does not need subsequent crushing treatment on the produced silicon dioxide, and is easy to realize industrial production.
Detailed Description
The present invention will be further described below by way of specific embodiments, but the present invention is not limited to only the following examples. Various modifications may be made by those skilled in the art based on the basic idea of the invention, but it is within the scope of the invention as long as it does not depart from the basic idea of the invention.
Example 1 preparation of high load high cleaning abrasive silica for dentifrice
The preparation method of the silicon dioxide for the high-load high-cleaning friction type dentifrice comprises the following steps:
s1, liquefying solid sodium silicate with the modulus of 3.5 at high temperature, and adding water to prepare a sodium silicate solution with the concentration of 3.0 mol/L;
s2, preparing a sulfuric acid solution with the concentration of 8.0 mol/L;
s3, adding 0.95 mass percent of sodium dodecyl sulfate solution into a reaction kettle, wherein the adding amount is 40 percent of the volume of the sodium silicate solution, heating to 85 ℃, opening a stirring paddle in the reaction kettle, setting the stirring frequency to be 40Hz, dropwise adding the sodium silicate solution prepared in the step S1 and the sulfuric acid solution prepared in the step S2 together under the stirring state, and the dropwise adding amount of the sodium silicate solution is 13.5m3The dropping speed of the sodium silicate solution is 5.0m3The dropping speed of the sulfuric acid solution is 3.0m3After the sodium silicate solution is dripped, controlling the reaction temperature to be 95 ℃, continuously dripping the sulfuric acid solution until the pH value in the reaction system is 5.5, continuously stirring and standing for 60min, and performing filter pressing to obtain a filter cake;
s4, washing the filter cake obtained in the step S3, spray-drying the obtained slurry, and controlling the particle size of the silicon dioxide to be 60 microns to obtain the silicon dioxide filter cake.
Example 2 preparation of high load high cleaning abrasive silica for dentifrice
The preparation method of the silicon dioxide for the high-load high-cleaning friction type dentifrice comprises the following steps:
s1, liquefying solid sodium silicate with the modulus of 2.5 at high temperature, and adding water to prepare a sodium silicate solution with the concentration of 2.6 mol/L;
s2, preparing a sulfuric acid solution with the concentration of 6.5 mol/L;
s3, adding 0.57 mass percent of sodium dodecyl sulfate solution into a reaction kettle, wherein the adding amount is 31 percent of the volume of the sodium silicate solution, heating to 83 ℃, opening a stirring paddle in the reaction kettle, setting the stirring frequency to be 36Hz, dropwise adding the sodium silicate solution prepared in the step S1 and the sulfuric acid solution prepared in the step S2 together under the stirring state, and the dropwise adding amount of the sodium silicate solution is 12.5m3The dropping speed of the sodium silicate solution is 4.3m3The dropping speed of the sulfuric acid solution is 2.5m3After the sodium silicate solution is dripped, controlling the reaction temperature to be 89 ℃, continuously dripping the sulfuric acid solution until the pH value in the reaction system is 4.5, continuously stirring and standing for 45min, and performing filter pressing to obtain a filter cake;
s4, washing the filter cake obtained in the step S3, spray-drying the obtained slurry, and controlling the particle size of the silicon dioxide to be 55 microns to obtain the silicon dioxide filter cake.
Example 3 preparation of high load high cleaning abrasive silica for dentifrice
The preparation method of the silicon dioxide for the high-load high-cleaning friction type dentifrice comprises the following steps:
s1, liquefying solid sodium silicate with the modulus of 1.5 at high temperature, and adding water to prepare a sodium silicate solution with the concentration of 1.5 mol/L;
s2, preparing a sulfuric acid solution with the concentration of 4.0 mol/L;
s3, adding 0.10% sodium dodecyl sulfate solution by mass into a reaction kettle, wherein the adding amount is 20% of the volume of the sodium silicate solution, heating to 70 ℃, opening a stirring paddle in the reaction kettle, setting the stirring frequency to be 30Hz, dropwise adding the sodium silicate solution prepared in the step S1 and the sulfuric acid solution prepared in the step S2 together under the stirring state, and the dropwise adding amount of the sodium silicate solution is 11.5m3The dropping speed of the sodium silicate solution is 3.5m3The dropping speed of the sulfuric acid solution is 2.0m3After the sodium silicate solution is dripped, controlling the reaction temperature to be 80 ℃, continuously dripping the sulfuric acid solution until the pH value in the reaction system is 3.5, continuously stirring and standing for 20min, and performing filter pressing to obtain a filter cake;
s4, washing the filter cake obtained in the step S3, spray-drying the obtained slurry, and controlling the particle size of the silicon dioxide to be 45 microns to obtain the silicon dioxide filter cake.
Comparative example 1 preparation of high load high cleaning abrasive silica for dentifrice
The high loading high cleaning abrasive dentifrice of the present comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: in this comparative example, sodium dodecylsulfate was not added in step S3.
Comparative example 2 preparation of high load high cleaning abrasive silica for dentifrice
The high loading high cleaning abrasive dentifrice of the present comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: in this comparative example, the reaction temperature was controlled to 65 ℃ after the completion of the dropwise addition of the sodium silicate solution in step S3.
Comparative example 3 preparation of high load high cleaning abrasive silica for dentifrice
The high loading high cleaning abrasive dentifrice of the present comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: the amount of sodium dodecyl sulfate added in step S3 of this comparative example was 10% by volume of the sodium silicate solution.
Comparative example 4 preparation of high load high cleaning abrasive silica for dentifrice
The high loading high cleaning abrasive dentifrice of the present comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: in this comparative example, the pH of the reaction system was controlled to 7.0 in step S3.
Test example I, Performance test
Test samples: silica for high loading high cleaning abrasive type dentifrice prepared in examples 1 to 3 and comparative examples 1 to 4;
the test method comprises the following steps: measuring the D50 particle size of a test sample by using a laser particle sizer (JX 93/M337792, Beijing, Western and Western technologies, Ltd.); detecting the water absorption capacity of the test sample by referring to GB/T32661-2016 spherical silica micropowder; the RDA values of the test materials were determined using a radioactive tracer method.
And (3) test results: the test results are shown in Table 1.
Table 1 results of performance testing
As can be seen from Table 1, the high-loading high-cleaning friction type silica for the dentifrice provided by the invention has the D50 particle size of 45-60 μm, the water absorption capacity of 120-180mL/100g, the RDA value of 116-135 and good friction performance and cleaning performance. Among these, the silica for high loading high cleaning abrasive dentifrice obtained in example 2 is the most excellent in all aspects and is the most preferred embodiment of the present invention.
Compared with the example 2, the addition amount of the sodium dodecyl sulfate is changed in the comparative example 1 and the comparative example 3, but the water absorption capacity of the prepared high-loading capacity high-cleaning friction type silicon dioxide for the dentifrice is greatly reduced, which fully indicates that the sodium dodecyl sulfate is beneficial to the aggregation and formation of primary particles and gradually surrounds to form macropores to form the characteristic of high adsorption of the silicon dioxide; comparative example 2 changed the system temperature after the addition of sodium silicate, but the average particle size of the obtained high loading force high cleaning friction type silica for dentifrice was reduced and the RDA value was greatly reduced, which indicates that friction type silica having a compact Shencheng structure was advantageous under high temperature conditions.
Test example two, application Performance test
Test samples: silica for high loading high cleaning abrasion type dentifrice obtained in examples 1 to 3, comparative example 1 and comparative example 3;
the test method comprises the following steps: a test sample is prepared into dentifrice according to the dentifrice formula, a blank control group adopts common silicon dioxide to replace the high-loading high-cleaning friction type silica dioxide for the dentifrice, the test sample is placed at normal temperature, the agglomeration condition of the dentifrice is observed at any time, and the time of the first agglomeration of the dentifrice is recorded.
The formula of the dentifrice is as follows: 15 parts of honeysuckle, 10 parts of sodium lauroyl sarcosinate, 4 parts of test sample, 4 parts of halite, 0.7 part of sodium carboxymethylcellulose, 0.9 part of xylitol, 0.4 part of essence, 0.3 part of butanediol and 30 parts of water.
The preparation method of the dentifrice comprises the following steps: pulverizing flos Lonicerae, cleaning, oven drying, adding sodium lauroyl sarcosinate and water, grinding, sieving, adding test sample, Halitum, sodium carboxymethylcellulose and silicon oxide, heating and stirring, sequentially adding xylitol, essence and butanediol, heating and stirring again, grinding, oven drying, and grinding again.
And (3) test results: the test results are shown in Table 2.
Table 2 application test results
| Group of | The time/day of occurrence of caking phenomenon |
| Example 1 | 87 |
| Example 2 | 93 |
| Example 3 | 91 |
| Comparative example 1 | 53 |
| Comparative example 3 | 49 |
| Blank control group | 32 |
As can be seen from Table 2, the silica for high loading force and high cleaning friction type dentifrice provided by the present invention can prevent moisture when applied to the dentifrice and prevent the dentifrice from absorbing moisture and agglomerating during storage. The agglomeration of the dentifrice prepared using the silica for high loading high cleaning abrasive dentifrice prepared in examples 1-3 was significantly increased compared to the blank control.
The above examples are merely illustrative of the preparation process of the present invention and do not limit the invention. Those skilled in the art will recognize that changes may be made to the embodiments described above without departing from the spirit and scope of the invention. Therefore, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the technical spirit of the present invention are covered by the claims of the present invention.
Claims (5)
1. A preparation method of silicon dioxide for high-loading capacity high-cleaning friction type dentifrice is characterized by comprising the following steps:
s1, liquefying solid sodium silicate at high temperature, and adding water to prepare a sodium silicate solution with the concentration of 1.5-3.0 mol/L;
s2, preparing a sulfuric acid solution with the concentration of 4.0-8.0 mol/L;
s3, adding the sodium dodecyl sulfate solution into the reaction kettle, heating to 70-85 ℃, opening a stirring paddle in the reaction kettle, and dropwise adding the sodium silicate solution prepared in the step S1 and the sulfuric acid solution prepared in the step S2 under the stirring state, wherein the dropwise adding amount of the sodium silicate solution is 11.5-13.5m3After the sodium silicate solution is dripped, controlling the reaction temperature to be 80-95 ℃, continuously dripping the sulfuric acid solution until the pH value in the reaction system is 3.5-5.5, continuously stirring, standing and press-filtering to obtain a filter cake;
s4, washing the filter cake obtained in the step S3, and spray-drying the obtained slurry to obtain the filter cake;
the modulus of the solid sodium silicate in the step S1 is 1.5-3.5; in the step S3, the mass percent of the sodium dodecyl sulfate solution is 0.10-0.95%, and the adding amount is 20-40% of the volume of the sodium silicate solution; the dropping speed of the sodium silicate solution in the step S3 is 3.5-5.0m3H; the dropping speed of the sulfuric acid solution is 2.0-3.0m3/h。
2. The method for preparing a silica for a high loading high cleaning abrasive dentifrice according to claim 1, wherein the stirring frequency of the stirring blade in the step S3 is 30 to 40 Hz.
3. The method for preparing a silica for a high loading high cleaning abrasion type dentifrice according to claim 1, wherein the standing time in the step S3 is 20 to 60 min.
4. The method for preparing a silica for a high loading high cleaning abrasion type dentifrice according to claim 1, wherein the particle size of the silica is controlled to be 45 to 60 μm during the spray drying in the step S4.
5. A high loading capacity high cleaning abrasive silica for dentifrice obtained by the process for producing the high loading capacity high cleaning abrasive silica according to any one of claims 1 to 4.
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