CN116891237A - Silicon dioxide as a toothpaste additive and its production process - Google Patents
Silicon dioxide as a toothpaste additive and its production process Download PDFInfo
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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
- 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
- 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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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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- 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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Abstract
The application relates to the technical field of toothpaste additives, and particularly discloses silicon dioxide serving as a toothpaste additive and a production process thereof. Firstly, mixing quartz sand and sodium carbonate, reacting for 4-6 hours at 1400-1600 ℃ to obtain a molten material, cooling to obtain a solid material, pressurizing to 0.4-1 MPa by using 100-150 ℃ water vapor, and spraying and dissolving the solid material to obtain a sodium silicate aqueous solution; heating the sodium silicate aqueous solution to 70-100 ℃, adding pentasodium aminotri (methylene phosphonic acid), adding acid and water under stirring after uniformly mixing to enable the final pH value of the solution to reach 2-4, filtering to obtain precipitate after white precipitate is generated in the process and is not separated out, washing the precipitate, then spray-drying the precipitate to obtain white powder, and finally baking the white powder at 150-200 ℃ to enable a small amount of non-decomposed silicic acid in the white powder to be completely decomposed into silicon dioxide, so as to obtain the silicon dioxide powder which is high in purity, good in uniformity and high in dispersibility and not easy to agglomerate.
Description
Technical Field
The application relates to the technical field of toothpaste additives, in particular to silicon dioxide serving as a toothpaste additive and a production process thereof.
Background
The main components of the general toothpaste comprise an abrasive, a humectant, a thickening agent, a surfactant, a flavoring agent and a medicament with therapeutic efficacy. Wherein the friction agent has the function of rubbing the tooth surface to remove dirt, and representative components are silicon dioxide, calcium hydrophosphate, calcium carbonate and the like. The thickener is used for binding other ingredients to form toothpaste with stable form, and the representative ingredients are silicon dioxide, sodium carboxymethyl cellulose, carbomer, etc.
The diameter of the silica particles for toothpaste should be 5-45 μm, the particle diameter is too large, and the toothpaste has obvious sand feel during brushing. The toothpaste body prepared by the friction agent with proper granularity has smooth and fine appearance and comfortable friction to the oral cavity and gum during tooth brushing. Too fine particle size (e.g., less than 1 μm) may cause thickening during storage of the toothpaste due to flocculation of the too fine abrasive during long-term storage of the toothpaste due to brownian motion.
Some toothpaste silica in the market has the problems of overlarge or undersize particle size, poor uniformity, easy caking and the like.
Disclosure of Invention
In order to solve the problems of overlarge or undersize particle size, poor uniformity and easy caking of silica for toothpaste in the market, the application provides silica serving as a toothpaste additive and a production process thereof.
In a first aspect, the present application provides a process for producing silica as an additive for toothpaste, and adopts the following technical scheme.
A process for producing silica as a toothpaste additive, the process comprising:
mixing quartz sand and sodium carbonate, reacting for 4-6 hours at 1400-1600 ℃ to obtain a molten state material, cooling to obtain a solid material, pressurizing to 0.4-1 MPa by using 100-150 ℃ water vapor, and spraying and dissolving the solid material to obtain a sodium silicate aqueous solution; heating the aqueous solution of sodium silicate to 70-100 ℃, adding pentasodium aminotri (methylene phosphonic acid), adding acid and water under stirring after uniformly mixing to enable the final pH value of the solution to reach 2-4, filtering to obtain precipitate after white precipitate is generated in the process and is not separated out, washing the precipitate, then spray-drying the precipitate to obtain white powder, and finally baking the white powder at 150-200 ℃ to obtain the silicon dioxide.
By adopting the technical proposal, quartz Sand (SiO) 2 ) And sodium carbonate (Na) 2 CO 3 ) Mixing, reacting for 4-6h at 1400-1600 ℃ to obtain molten sodium silicate, and reacting at the temperature to obtain sodium silicate with low impurity content. The sodium silicate becomes solid after cooling, and can be loaded in a rotary spherical digester, pressurized to 0.4-1 MPa by high-temperature steam with the temperature of 100-150 ℃ and dissolved to form colorless transparent viscous liquid, namely sodium silicate aqueous solution. Heating the sodium silicate aqueous solution to 70-100 ℃, adding pentasodium aminotri (methylene phosphonic acid), uniformly mixing, and then adding acid and water under stirring to enable the final pH value of the solution to reach 2-4, wherein the acid can be sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid and the like, the sodium silicate reacts with the acid to generate silicic acid, the aqueous solution is heated to 70-100 ℃, and the stability of the reaction rate is maintained. The pentasodium aminotri (methylene phosphonic acid) is easy to dissolve in water, can form hydrogen bonds with silicic acid on the first aspect to prevent excessive aggregation of silicic acid, and on the second aspect, because the pentasodium aminotri (methylene phosphonic acid) molecular chain is short and three-dimensional, the wrapping property of silicic acid is moderate, the diameter of microparticles aggregated by silicic acid is proper, and the pentasodium aminotri (methylene phosphonic acid) can not be too large or too small. And after acid is added, white precipitate is separated out to be silicic acid, and at the moment, pentasodium aminotri (methylene phosphonic acid) and the silicic acid are completely desorbed, so that the desorption efficiency is high. The silicic acid is decomposed into silicon dioxide by heating, and the precipitated silicon dioxide has uniform particle size, high purity and good whiteness. The final pH of the solution reaches 2-4, so that excessive sodium carbonate can be reacted, ionization of silicic acid can be prevented, ionization balance is converted to a molecular state, silicic acid molecules are easy to be heated and decomposed to separate out silicon dioxide, if the pH is too low, the solubility of silicic acid is high, silicon dioxide is not easy to separate out, and if the pH is too high, ionization balance is converted to an ionic state, and silicon dioxide is not easy to separate out. After the white precipitate is no longer precipitated, the silicic acid/silicon dioxide is no longer precipitated, white powder is obtained through filtration, washing and spray drying,the white powder is baked at the temperature of 150-200 ℃ to ensure that a small amount of non-decomposed silicic acid in the white powder is completely decomposed into silicon dioxide, thus obtaining the silicon dioxide powder with high purity, good uniformity and high dispersibility and difficult caking.
Optionally, the mass ratio of the sodium carbonate to the quartz sand is 1: (1.5-3.5).
By adopting the technical proposal, sodium carbonate and quartz sand react for 4 to 6 hours at 1400 to 1600 ℃ to obtain molten sodium silicate with the molecular formula of Na 2 O·nSiO 2 According to the proportion of the added sodium carbonate and quartz sand, the modulus n is 1.5-3.5, sodium silicate generated when n is too large is not easy to dissolve in water, is not easy to be dissolved by water vapor, and also affects the subsequent reaction with acid and the particle size concentration of the generated silicon dioxide, and the consumption of sodium carbonate is increased when n is too small.
Optionally, the mass ratio of the sodium carbonate to the quartz sand is 1:3.
by adopting the technical scheme, the generated sodium silicate has high purity, high efficiency of being dissolved by high-temperature steam and small sodium carbonate consumption.
Optionally, the mass ratio of the quartz sand to the pentasodium aminotri (methylenephosphonic acid) is 1: (0.01-0.03).
By adopting the technical scheme, sodium silicate is generated by the quartz sand and sodium carbonate, and in the process of generating silicic acid by the reaction of sodium silicate and acid, hydrogen bonds are formed between aminotri (methylene phosphonic acid) pentasodium and silicic acid to prevent excessive aggregation of silicic acid, so that the size of aggregated silicic acid particles is controlled within the range of 23-45 mu m, and the silicon dioxide has better grinding effect and thickening effect when being applied to toothpaste.
Optionally, the mass ratio of the quartz sand to the pentasodium aminotri (methylenephosphonic acid) is 1:0.02.
by adopting the technical scheme, sodium silicate is generated by the quartz sand and sodium carbonate, and in the process of generating silicic acid by the reaction of sodium silicate and acid, hydrogen bonds are formed between aminotri (methylene phosphonic acid) pentasodium and silicic acid to prevent excessive aggregation of silicic acid, so that the proportion of silicic acid aggregation particles in the range of 33-38 mu m is obviously increased, the particle size uniformity is high, caking is not easy to occur, and the silicon dioxide has better grinding effect and thickening effect when being applied to toothpaste.
Optionally, adding acid and water under the stirring condition, and adjusting the final pH of the aqueous solution to be 2.8-3.2.
By adopting the technical scheme, the silicic acid basically exists in a solution in a molecular state and is extremely easy to be decomposed into silicon dioxide by heating, so that highly dispersed silicon dioxide particles are obtained, the particle size is mostly in a uniform range of 23-45 mu m, and the proportion can reach more than 30% in a range of 33-38 mu m.
Optionally, mixing the quartz sand and the sodium carbonate, and reacting for 4.8-5.2 hours at 1550-1560 ℃ to obtain the molten material.
By adopting the technical scheme, the purity of sodium silicate generated by the reaction of quartz sand and sodium carbonate is high in the temperature range, and the purity of the subsequently produced silicon dioxide is correspondingly improved to more than 98%.
Optionally, the volume of the sodium silicate aqueous solution is V, the flow of the added acid is V/(20-40) per minute, and the stirring speed is kept at 200-300 r/min in the acid adding process.
By adopting the technical scheme, the acid adding speed and the stirring speed are controlled, so that the dispersibility and the granularity uniformity of the generated silicic acid are improved.
Optionally, heating the aqueous solution of sodium silicate to 84-86 ℃, adding pentasodium aminotri (methylenephosphonic acid), mixing uniformly, and adding acid and water under stirring.
By adopting the technical scheme, at the temperature, the activity of the pentasodium aminotri (methylene phosphonic acid) is strong, and the hydrogen bond effect generated by silicic acid is large, so that the silicic acid has proper particle size and uniform dispersion.
In a second aspect, the application also provides silica as an additive for toothpaste, and adopts the following technical scheme.
Silica as an additive for toothpaste is prepared according to the above-mentioned production process.
By adopting the technical scheme, the silicon dioxide which has proper particle size, good uniformity and difficult caking and is suitable for being used as a toothpaste friction agent and a thickening agent simultaneously is prepared.
In summary, the silica serving as the toothpaste additive and the production process thereof have the following beneficial effects:
by controlling the reaction temperature between 1400 and 1600 ℃, the quartz sand (SiO 2 ) And sodium carbonate (Na) 2 CO 3 ) The molten sodium silicate is obtained by the reaction, and the impurity content of the sodium silicate obtained by the reaction at the temperature is low.
The solid sodium silicate can be efficiently dissolved by using high-temperature steam with the temperature of 100-150 ℃ and pressurizing to 0.4-1 MPa, so as to form colorless transparent viscous liquid, namely sodium silicate aqueous solution.
Heating the sodium silicate aqueous solution to 70-100 ℃, adding pentasodium aminotri (methylene phosphonic acid), uniformly mixing, adding acid and water under stirring, and reacting the sodium silicate and the acid to generate silicic acid. Wherein, the aqueous solution is heated and kept at 70-100 ℃ to keep the stability of the reaction rate. The amino tri (methylene phosphonic acid) pentasodium can form hydrogen bond with silicic acid to prevent excessive aggregation of silicic acid, and the amino tri (methylene phosphonic acid) pentasodium molecular chain is short and three-dimensional, so that the coating property of silicic acid is moderate, the diameter of microparticles formed by aggregation of silicic acid is proper and cannot be too large or too small, and in the third aspect, the density of amino tri (methylene phosphonic acid) pentasodium is more than 1.4g/cm 3 The density of the aqueous solution can be moderately increased, the interfacial tension of the silicic acid particles and water is reduced, the dispersion of the particles is facilitated, the silicic acid particles are suspended in the aqueous solution, the silicic acid particles are prevented from settling and gathering too fast, and the silicic acid particles are uniformly dispersed. The silicic acid is decomposed into silicon dioxide by heating, and the precipitated silicon dioxide has uniform particle size, high purity and good whiteness.
Adding acid, reacting sodium silicate with the acid to generate silicic acid, controlling the final pH value of the solution to be 2-4, not only reacting excessive sodium carbonate, but also preventing ionization of the silicic acid, wherein ionization balance is changed to a molecular state, silicic acid molecules are easy to be heated to decompose and separate out silicon dioxide, if the pH value is too low, the solubility of the silicic acid is high, silicon dioxide is not easy to separate out, and if the pH value is too high, ionization balance is changed to an ionic state, and silicon dioxide is not easy to separate out.
Finally, baking the white powder obtained by spray drying at the temperature of 150-200 ℃ to ensure that a small amount of non-decomposed silicic acid in the white powder is completely decomposed into silicon dioxide, thus obtaining the silicon dioxide powder with high purity, good uniformity and high dispersibility and difficult caking.
Detailed Description
Some examples of the silica as a toothpaste additive and its production process according to the present application are specifically described below. The mass of the following materials has been converted into relative parts by mass.
Example 1
Mixing 3 parts of quartz sand and 1 part of sodium carbonate, reacting for 5 hours at 1555 ℃ to obtain molten sodium silicate, cooling to obtain solid sodium silicate, pressurizing to 0.4MPa by using 125 ℃ of water vapor, and spraying and dissolving the sodium silicate to obtain sodium silicate aqueous solution with the volume of V; heating the aqueous solution of sodium silicate at 85 ℃, adding 0.02 part of pentasodium aminotri (methylene phosphonic acid), uniformly mixing, adding sulfuric acid and water under stirring, wherein the flow rate of the added sulfuric acid is V/30 per minute, maintaining the stirring speed at 250 revolutions per minute in the process of adding sulfuric acid, controlling the amount of the added sulfuric acid to enable the final pH value of the solution to reach 3, filtering to obtain a precipitate after white precipitate is generated in the process and is not separated out, washing the precipitate, then spray-drying the precipitate to obtain white powder, and finally baking the white powder at 150 ℃ to obtain the silicon dioxide.
Example 2
The only difference between this example and example 1 is that 3.5 parts of quartz sand was added, the solid was sprayed and dissolved by pressurizing to 1MPa with steam at 125 c, the dissolution time was 16% higher than that of example 1 under the same conditions, and an aqueous sodium silicate solution was obtained after dissolution, and finally silica was prepared.
Example 3
The only difference between this example and example 1 is that 0.01 part of pentasodium aminotri (methylenephosphonic acid) was added and finally a silica was prepared.
Example 4
The only difference between this example and example 1 is that 0.03 parts of pentasodium aminotri (methylenephosphonic acid) was added and finally a silica was prepared.
Example 5
The only difference between this example and example 1 is that the amount of sulfuric acid added is controlled so that the final pH of the solution reaches 2, and finally silica is produced.
Example 6
The only difference between this example and example 1 is that the amount of sulfuric acid added is controlled so that the final pH of the solution reaches 4, and finally silica is produced.
Example 7
The only difference between this example and example 1 is that silica was prepared by mixing silica sand and soda ash and then reacting at 1400℃for 5 hours to obtain molten sodium silicate.
Example 8
The only difference between this example and example 1 is that silica was prepared by mixing silica sand and soda ash and reacting at 1600 c for 5 hours to obtain molten sodium silicate.
Example 9
The only difference between this example and example 1 is that the aqueous sodium silicate solution was heated to 70 c and pentasodium aminotri (methylenephosphonic acid) was added to finally prepare silica.
Comparative example 1
The only difference between this comparative example and example 1 is that pentasodium aminotri (methylenephosphonic acid) was not added and finally a silica was prepared.
Comparative example 2
The only difference between this comparative example and example 1 is that 0.02 parts of sodium dodecylbenzenesulfonate was added to finally prepare silica.
Comparative example 3
The only difference between this comparative example and example 1 is that 0.02 parts of sodium dodecyl sulfate was added and finally a silica was prepared.
Comparative example 4
The only difference between this comparative example and example 1 is that the amount of sulfuric acid added is controlled so that the final pH of the solution reaches 1, and finally silica is produced.
Comparative example 5
The only difference between this comparative example and example 1 is that the amount of sulfuric acid added is controlled so that the final pH of the solution reaches 5, and finally silica is produced.
Comparative example 6
The only difference between this comparative example and example 1 is that silica was prepared by mixing silica sand and soda ash and then reacting at 1300℃for 5 hours to obtain molten sodium silicate.
Comparative example 7
The only difference between this comparative example and example 1 is that the aqueous sodium silicate solution was heated to 50 c and pentasodium aminotri (methylenephosphonic acid) was added to finally prepare silica.
Comparative example 8
The only difference between this comparative example and example 1 is that the flow of sulfuric acid was V/10 per minute, and finally silica was produced.
Test example 1
The silica prepared in examples 1-9 and comparative examples 1-8 were tested according to QB/T2346-2007 Standard for silica tests for toothpastes. The test results are shown in Table 1.
Table 1 results of silica property test prepared in each of examples and comparative examples
The test was conducted using a 600 mesh sieve (passing through particle size 23 μm), a 425 mesh sieve (passing through particle size 33 μm), a 400 mesh sieve (passing through particle size 38 μm) and a 325 mesh sieve (passing through particle size 45 μm) for increasing the particle size of silica prepared in each of examples and comparative examples, and the results are shown in Table 2 below.
Table 2 silica particle size detection prepared in each example and comparative example
From tables 1 and 2 above, it can be seen that the particle size concentration of examples 1 to 9 is significantly improved, the proportion in the range of 23 to 45 μm can be more than 70%, and the proportion in the range of 33 to 38 μm can be more than 30%, compared with the silica prepared in comparative examples 1 to 8. When the diameter of the silica particles is 23-45 mu m, even 33-38 mu m, the silica particles are not easy to adhere, have good friction property when being applied to toothpaste, are not easy to damage teeth, have thickening effect on the toothpaste, and enable the toothpaste to have elasticity and shape retention under low shearing force.
Example 1 has the best particle size concentration and purity compared to the other examples.
In example 2, the amount of silica sand was increased as compared with example 1, and the particle size concentration was somewhat decreased.
Examples 3 and 4, in which the addition ratio of pentasodium aminotri (methylenephosphonic acid) was adjusted as compared to example 1, examples 5 and 6, in which the final pH of the solution was adjusted as compared to example 1, had both a slight decrease in silica purity and particle size concentration.
Compared with example 1, the melting reaction temperature of quartz sand and sodium carbonate is reduced to 1400 ℃, the purity of the finally prepared silicon dioxide is reduced by 1.5%, and the reduction of the particle size concentration is not obvious.
Example 8 compared to example 1, the silica prepared by increasing the temperature of the fused silica sand and soda ash to 1600 ℃ had a purity and particle size concentration comparable to example 1.
Example 9 compared with example 1, the temperature of the aqueous sodium silicate solution is reduced from 85 ℃ to 70 ℃, the purity of the finally prepared silicon dioxide is reduced by 1.1%, the particle size concentration is also obviously reduced, and the reaction temperature has obvious influence on the reaction of sodium silicate and sulfuric acid and the dispersing effect of pentasodium aminotri (methylenephosphonic acid).
Comparative example 1 compared with example 1, no pentasodium aminotri (methylenephosphonic acid) was added, and finally the silica prepared had a higher proportion of particles size range dispersion, both less than 23 μm and greater than 45 μm.
Comparative example 2 compared with example 1, the use of sodium dodecyl benzene sulfonate instead of pentasodium aminotri (methylenephosphonic acid) finally produced silica with a significant increase in dry agent burn weight loss ratio at 900 ℃ which may be less likely to be washed clean after the combination of sodium dodecyl benzene sulfonate and silicic acid, resulting in residual effects.
Comparative example 3 compared with example 1, the use of sodium dodecyl sulfonate instead of pentasodium aminotri (methylenephosphonic acid) finally produced silica with a significant increase in dry agent burn weight loss ratio at 900 ℃, which may be less likely to be washed clean after the combination of sodium dodecyl benzene sulfonate and silicic acid, resulting in residual effects.
Comparative example 4 and comparative example 5 have the effect of adjusting the final pH of the solution, affecting the dispersing effect of silicic acid, and have a certain decrease in the particle size concentration of silica, compared with example 1.
Compared with the comparative example 6, the melting reaction temperature of quartz sand and sodium carbonate is reduced to 1300 ℃, the purity of the finally prepared silicon dioxide is reduced by 3.3%, the concentration of the particle size is also reduced to a certain extent, and the excessively low temperature is unfavorable for removing impurities.
Comparative example 7 compared with example 1, the heating of the aqueous sodium silicate solution was reduced from 85 to 50 c, the particle size concentration of silica was significantly reduced, and it was found that the reaction temperature had a certain effect on the dispersing effect.
Compared with the example 1, the flow rate of sulfuric acid is increased from V/30 to V/10 per minute, and the concentration of the particle size of the finally prepared silicon dioxide is reduced to a certain extent, which shows that the excessively rapid sulfuric acid addition rate has a certain destructive effect on the dispersion of the generated silicic acid.
In summary, by controlling the silica sand (SiO 2 ) And sodium carbonate(Na 2 CO 3 ) The melting reaction temperature is 1400-1600 ℃, and the impurity content of sodium silicate obtained by the reaction is low.
The reaction temperature of sodium silicate and sulfuric acid is kept between 70 and 100 ℃, the final pH of the solution is controlled to be 2 to 4, and the aminotri (methylene phosphonic acid) pentasodium added in the reaction has remarkable effect on the uniform dispersion of the silicon dioxide of the final product to form proper particle size. Finally, baking the white powder obtained by spray drying at the temperature of 150-200 ℃ to ensure that a small amount of non-decomposed silicic acid in the white powder is completely decomposed into silicon dioxide, thus obtaining the silicon dioxide powder with high purity, good uniformity and high dispersibility and difficult caking.
The above is merely a preferred embodiment of the present application, the protective scope of the present application is not limited to the above examples, it should be noted that modifications and alterations will be apparent to those skilled in the art without departing from the principle of the present application, and these modifications and alterations should also be regarded as falling within the protective scope of the present application.
Claims (10)
1. A process for producing silica as a toothpaste additive, the process comprising:
mixing quartz sand and sodium carbonate, reacting for 4-6 hours at 1400-1600 ℃ to obtain a molten material, cooling to obtain a solid material, pressurizing to 0.4-1 MPa by using 100-150 ℃ water vapor, and spraying and dissolving the solid material to obtain a sodium silicate aqueous solution; heating the sodium silicate aqueous solution to 70-100 ℃, adding pentasodium aminotri (methylene phosphonic acid), adding acid and water under stirring after uniformly mixing to enable the final pH value of the solution to reach 2-4, filtering to obtain a precipitate after white precipitate is generated in the process and is not separated out, washing the precipitate, then spray-drying the precipitate to obtain white powder, and finally baking the white powder at 150-200 ℃ to obtain the silicon dioxide.
2. The process for producing silica as an additive for toothpaste according to claim 1, wherein the mass ratio of the soda ash to the silica sand is 1: (1.5 to 3.5).
3. The process for producing silica as a toothpaste additive according to claim 2, wherein the mass ratio of the soda ash to the silica sand is 1:3.
4. the process for producing silica as a toothpaste additive according to claim 1, wherein the mass ratio of the quartz sand to the aminotri (methylenephosphonic acid) pentasodium is 1: (0.01 to 0.03).
5. The process for producing silica as a toothpaste additive according to claim 4, wherein the mass ratio of the quartz sand to the aminotri (methylenephosphonic acid) pentasodium is 1:0.02.
6. the process for producing silica as an additive for toothpaste according to claim 1, wherein the acid and water are added under stirring, and the final pH of the aqueous solution is adjusted to 2.8 to 3.2.
7. The process for producing silica as claimed in claim 1, wherein the silica sand and the soda ash are mixed and reacted at 1550-1560 ℃ for 4.8-5.2 hours to obtain the molten material.
8. The process for producing silica as claimed in claim 1, wherein the volume of the aqueous sodium silicate solution is V, the flow rate of the acid is V/(20-40) per minute, and the stirring speed is maintained at 200-300 rpm during the acid addition.
9. The process for producing silica as claimed in claim 1, wherein the aqueous solution of sodium silicate is heated to 84-86 ℃, pentasodium aminotri (methylenephosphonic acid) is added thereto, and the acid and water are added under stirring after being uniformly mixed.
10. Silica as toothpaste additive, characterized in that it is prepared according to the production process of any one of claims 1-9.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN103539129A (en) * | 2013-10-30 | 2014-01-29 | 武汉大学 | Purification method of silicon dioxide |
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| WO2023035097A1 (en) * | 2021-09-07 | 2023-03-16 | 无锡恒诚硅业有限公司 | Preparation method for particle size-controllable white carbon black |
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| US5000933A (en) * | 1989-01-31 | 1991-03-19 | Henkel Kommanditgesellschaft Auf Aktien | Process for hydrothermal production of sodium silicate solutions |
| KR20000016390A (en) * | 1996-06-06 | 2000-03-25 | 트롤리에 모리스, 다니엘 델로스 | Silica capable of being used in toothpaste compositions |
| JP3691048B1 (en) * | 2004-08-09 | 2005-08-31 | 日本化学工業株式会社 | Method for producing high purity colloidal silica |
| WO2007042640A1 (en) * | 2005-10-06 | 2007-04-19 | Rhodia Recherches Et Technologies | Silicas comprising phosphonic-acid-modified surfaces |
| US8512664B1 (en) * | 2007-07-20 | 2013-08-20 | The National Titanium Dioxide Co. Ltd. (Cristal) | Sodium silicate solutions |
| JP2015020916A (en) * | 2013-07-16 | 2015-02-02 | ケイ・エス・ティ・ワ−ルド株式会社 | Method for manufacturing high-purity synthetic silica powder |
| CN103435048A (en) * | 2013-08-17 | 2013-12-11 | 福建省三明同晟化工有限公司 | Preparation method of silicon dioxide used for tooth paste |
| CN103539129A (en) * | 2013-10-30 | 2014-01-29 | 武汉大学 | Purification method of silicon dioxide |
| WO2023035097A1 (en) * | 2021-09-07 | 2023-03-16 | 无锡恒诚硅业有限公司 | Preparation method for particle size-controllable white carbon black |
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