CN110342527A - A kind of low partial size high dispersive high transparent toothpaste silica and preparation method thereof - Google Patents
A kind of low partial size high dispersive high transparent toothpaste silica and preparation method thereof 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
- A61K8/18—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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- 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
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- 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
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Abstract
The invention belongs to Silica Using for Toothpaste technical fields, and in particular to a kind of low partial size high dispersive high transparent toothpaste silica and preparation method thereof.Preparation method of the present invention includes: S1, polyethylene glycol is added into sodium silicate solution, and solution is dispersed with stirring uniformly, obtains sodium metasilicate mixed solution;S2, metabisulfite solution is added into reactor tank, opens stirring, heating;S3, under stiring, while sodium metasilicate mixed solution and sulfuric acid solution is added dropwise, control pH value is 8.5~9.5, controls temperature, after sodium metasilicate mixed solution is added, continues that sulfuric acid solution is added dropwise, when pH is 4.0~5.0, stops acid adding, obtain silica;S4, obtained silica carries out to filters pressing, washing, by obtaining Silica Using for Toothpaste after spray drying treatment, this method simple process, silica partial size obtained is small, good dispersion, light transmittance are high, meets the applications well in toothpaste.
Description
Technical field
The invention belongs to silica preparation technical fields, and in particular to a kind of low partial size high dispersive high transparent toothpaste is with two
Silica and preparation method thereof.
Background technique
Silica is because its physics and chemical property are highly stable, acid and alkali-resistance high temperature resistant, no pollution to the environment, has good
Clean-up performance, frictional force, and not damage tooth, and good with the material combination in toothpaste, fluorine compatibility is high, thus replaces carbon
Abrasive material and thickener of the other raw materials such as sour calcium as toothpaste.
Currently, the Silica Using for Toothpaste particle of precipitation method preparation, is primarily present following problems:
One, silica partial size is excessive, reaches 20~40 μm, and needing to carry out break process to partial size is 8~15 μm,
It is able to satisfy the applications well in toothpaste, not only results in that the production cost increases in this way, is also easy to destroy the pattern of particle itself,
Original performance of product is reduced, and will cause the waste of product.
Two, the apparent activation energy of silicon dioxide granule is higher, and interaction is easy between particle, is formed and is reunited, caused point
Dissipate performance decline.
Three, the light transmittance of silica is relatively low, so that the light transmittance of the liquid-phase system of lotion and solid system difference is larger,
It is difficult to obtain the high toothpaste of transparency.
Therefore, the performance for how effectively improving precipitated silica becomes the emphasis studied at present.
If patent document CN109607555A discloses a kind of preparation method of high friction high transparent toothpaste silica,
This method comprises: S1, metabisulfite solution is added into reactor tank, it is warming up to 60~65 DEG C;S2, to be added with stirring sodium metasilicate molten
It is warming up to 60~65 DEG C after liquid, sulfuric acid solution is added dropwise, when pH value is 8.5~9.5, stops acid adding, ageing;S3, it is added simultaneously
Sodium silicate solution and sulfuric acid solution are reacted, and control process pH value is 8.0~9.0, after sodium silicate solution adds, are continued
It is 4.5~5.0 that sulfuric acid solution to pH value, which is added dropwise,;S4, the silica of formation is subjected to filters pressing, washed, spray drying, air-flow is broken
It is broken, obtain silica.The light transmittance for the silica that this method obtains is high, and transparency is good, is suitably applied transparent toothpaste
Preparation, but the initial particle of the silica is big, needs to carry out air-flow break process, production cost is caused to increase, product is former
There is reduced performance.
For another example patent document CN107892306A discloses a kind of preparation of low partial size high water absorption Silica Using for Toothpaste
Method, comprising: the first step, prepare modulus be 1~3, the waterglass that concentration is 1.5~3.0M, be warming up to 80~100 DEG C, open
Stirring;Second step, compound concentration sulfuric acid solution are added sodium pyrophosphate and dodecyl dimethyl benzyl ammonium bromide, solution are stirred
It mixes and is uniformly dispersed, obtain sulfuric acid mixed solution;Third step starts dropwise addition into the water glass solution for being warming up to 80~100 DEG C
The resulting sulfuric acid mixed solution of two steps controls reaction end pH4~6, stirring ageing 0.5h;4th step, the titanium dioxide by formation
Silicon carries out filters pressing, washing, carries out spray drying treatment again to obtain partial size being 8~15 μm of silica products.This method can obtain
The silica that particle diameter distribution is low, dispersibility is high is obtained, but the reaction temperature of this method is high, and needs using sodium pyrophosphate and ten
Dialkyl dimethyl Benzylphosphonium Bromide ammonium leads to complex process, at high cost, is unfavorable for promoting and applying as reaction promoter.
In summary, it is necessary to research and develop a kind of preparation method of silica, this method simple process, and can improve simultaneously
Partial size, dispersibility and the light transmittance of silica.
Summary of the invention
In order to overcome problems of the prior art, the present invention provides a kind of low partial size high dispersive high transparent toothpastes to use
Silica and preparation method thereof, this method simple process, using polyethylene glycol as auxiliary agent, by a step hydrothermal deposition method,
The partial size of silica obtained is small, good dispersion, light transmittance are high, meets the applications well in toothpaste.
Present invention firstly provides the preparation methods of low partial size high dispersive high transparent toothpaste silica, including following step
It is rapid:
S1, polyethylene glycol is added into sodium silicate solution, solution is dispersed with stirring uniformly, obtain sodium metasilicate mixed solution;
S2,10~12m of metabisulfite solution is added into reactor tank3, stirring is opened, is warming up to 70~75 DEG C;
S3, stirring is lower while 8~10m of sodium metasilicate mixed solution is added dropwise3And sulfuric acid solution, control sodium metasilicate mixed solution
Flow velocity is 13~14m3/ h, reaction process pH value are 8.5~9.5, and reaction temperature is 70~75 DEG C, when sodium metasilicate mixed solution
After addition, continue that sulfuric acid solution is added dropwise, when pH is 4.0~5.0, stops acid adding, obtain silica;
S4, the silica of formation is carried out to filters pressing, washing, by obtaining low partial size high dispersive after spray drying treatment
High transparent toothpaste silica.
Further, the concentration of the sodium silicate solution is 2.0~3.5mol/L.
Further, the molecular weight of the polyethylene glycol is 4000~6000.
Further, the additional amount of the polyethylene glycol is 4~8wt% of sodium silicate solution.
Further, the mass percent concentration of the metabisulfite solution is 4.0~6.0%.
Further, the concentration of the sulfuric acid solution is 8~10mol/L.
Further, the flow velocity of the sulfuric acid solution is 2.5~3.5m3/h。
Further, the frequency of the stirring is 25~35Hz.
Correspondingly, the present invention also provides the preparation methods by above-mentioned low partial size high dispersive high transparent toothpaste silica
Obtained silica, the partial size of the silica are 8~15 μm, disperse the silica in 70% sorbitol solution
In, it observes after being sufficiently stirred, the uniform soilless sticking of system, by visible spectrophotometer test system light transmittance >=93%, uses
The silica makes toothpaste, and after placing six months under room temperature, toothpaste still keeps transparent light, and lotion is not reunited, and first
Beginning appearance is no different.
The present invention prepares low partial size high dispersive high transparent toothpaste silica, and the reaction mechanism is as follows:
The present invention uses a step hydrothermal deposition method, using polyethylene glycol as reaction promoter, and is added in sodium silicate solution and joins
With react, with metabisulfite solution be reaction bottom liquid, dripped under high-speed stirred and relatively low reaction temperature, while into bottom liquid
Add sodium metasilicate mixed solution and the concentrated sulfuric acid, and the temperature for controlling reaction process is 70~75 DEG C, pH value is 8.5~9.5, so that just
The loose gel particles that begin quickly are formed, and the characteristic that the crystal seed that this single step reaction generates has light transmittance high is dripping silicic acid
Continue that the concentrated sulfuric acid is added dropwise on the basis of sodium mixed solution, with the addition of the concentrated sulfuric acid, crystal seed continued growth tends to certain partial size
Uniformly.
Meanwhile during the reaction, because polyethylene glycol is nonionic surface active agent, it is in silica dioxide granule table
Face absorption, silica particle surface combination water is gradually replaced by polyethylene glycol polymer, in conjunction with water in silicon dioxide granule table
The Percentage bound in face declines, and so that silica particle surface is reduced, growing up for particle can be prevented, along with polyethylene glycol long chain
Mutually winding can promote micelle cohesion, interacts and weakens between particle, dispersibility improves, so that silica partial size is equal
One, it tends towards stability.
It is worth noting that, in the present invention, need to select molecular weight is 4000~6000 polyethylene glycol, this is because working as
When the molecular weight of polyethylene glycol is greater than 6000, silicon dioxide granule is easy to be wrapped up by the polyethylene glycol of macromolecule, surface-active
The decline of hydroxyl quantity, is unfavorable for the growth of particle;And when molecular weight is less than 4000, silicon dioxide granule during the growth process,
Because small-molecular-weight polyethylene glycol function and effect weaken, surface-active hydroxyl quantity increases, in conjunction with water in silicon dioxide granule table
The Percentage bound in face increases, and partial size problems of too occurs in particle continued propagation, and the later period will carry out break process.
Therefore, compared with prior art, present invention has an advantage that
(1) particle diameter distribution of the low partial size high dispersive high transparent toothpaste silica of the present invention is 8~15 μm, simultaneously will
Silica is scattered in 70% sorbitol solution, is observed after being sufficiently stirred, and particle is uniform, is had high dispersive characteristic, is passed through
Visible spectrophotometer test system light transmittance >=93%, it can be seen that the silica is fully met as toothpaste auxiliary agent
The requirement applied in toothpaste has good market prospects.
(2) preparation method of the low partial size high dispersive high transparent toothpaste silica of the present invention by adding in the reaction system
Addition polymerization ethylene glycol, while temperature, pH value, material concentration and the reaction time etc. for controlling reaction process, have silica
The characteristic of low partial size, high dispersive and high transparency, and the simple process of the method for the present invention, stabilization, condition is easily-controllable, needs not move through brokenly
Broken processing, reduces production cost, reduces energy consumption.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1, the low partial size high dispersive high transparent toothpaste silica of the present invention and preparation method thereof
The polyethylene glycol that molecular weight is 4000, polyethylene glycol are added in S1, the sodium silicate solution for being 2.0mol/L to concentration
Additional amount be sodium silicate solution 4wt%, be dispersed with stirring uniformly, obtain sodium metasilicate mixed solution;
S2, the metabisulfite solution 10m that mass percent concentration is 4.0% is added into reactor tank3, setting stirring unit frequency
For 25Hz, stirring is opened, is warming up to 70 DEG C;
S3, stirring is lower while sodium metasilicate mixed solution 8m is added dropwise3It is carried out in cocurrent with concentration for the sulfuric acid solution of 8mol/L
And reaction, the flow velocity of control sodium metasilicate mixed solution are 13m3/ h, sulfuric acid solution flow velocity be 2.5m3/ h, reaction process pH value are
8.5, reaction temperature is 70 DEG C, after sodium metasilicate mixed solution is added, continues that sulfuric acid solution is added dropwise, when pH is 4.0, stop
Only acid adding obtains silica;
S4, obtained silica is carried out to filters pressing, washing, by obtaining low partial size high dispersive after spray drying treatment
High transparent toothpaste silica.
Embodiment 2, the low partial size high dispersive high transparent toothpaste silica of the present invention and preparation method thereof
The polyethylene glycol that molecular weight is 6000, polyethylene glycol are added in S1, the sodium silicate solution for being 3.5mol/L to concentration
Additional amount be sodium silicate solution 8wt%, be dispersed with stirring uniformly, obtain sodium metasilicate mixed solution;
S2, the metabisulfite solution 12m that mass percent concentration is 6.0% is added into reactor tank3, setting stirring unit frequency
For 35Hz, stirring is opened, is warming up to 70 DEG C;
S3, stirring is lower while sodium metasilicate mixed solution 10m is added3With the sulfuric acid solution progress cocurrent that concentration is 10mol/L
Neutralization reaction, the flow velocity of control sodium metasilicate mixed solution are 13m3/ h, sulfuric acid solution flow velocity be 3.5m3/ h, reaction process pH value
Be 9.5, reaction temperature be 70 DEG C, when sodium metasilicate mixed solution be added after, continue be added dropwise sulfuric acid solution, when pH value be 5.0,
Stop acid adding, obtains silica;
S4, obtained silica is carried out to filters pressing, washing, by obtaining low partial size high dispersive after spray drying treatment
High transparent toothpaste silica.
Embodiment 3, the low partial size high dispersive high transparent toothpaste silica of the present invention and preparation method thereof
The polyethylene glycol that molecular weight is 6000, polyethylene glycol are added in S1, the sodium silicate solution for being 2.2mol/L to concentration
Additional amount be sodium silicate solution 6wt%, be dispersed with stirring uniformly, obtain sodium metasilicate mixed solution;
S2, the metabisulfite solution 10m that mass percent concentration is 4.5% is added into reactor tank3, setting stirring unit frequency
For 30Hz, stirring is opened, is warming up to 75 DEG C;
S3, stirring is lower while sodium metasilicate mixed solution 10m is added3It is carried out in cocurrent with concentration for the sulfuric acid solution of 8mol/L
And reaction, the flow velocity of control sodium metasilicate mixed solution are 14m3/ h, sulfuric acid solution flow velocity be 3.5m3/ h, reaction process pH value are
9.0, reaction temperature be 75 DEG C, when sodium metasilicate mixed solution be added after, continue be added dropwise sulfuric acid solution, when pH value be 4.8, stop
Only acid adding obtains silica;
S4, obtained silica is carried out to filters pressing, washing, by obtaining low partial size high dispersive after spray drying treatment
High transparent toothpaste silica.
Embodiment 4, the low partial size high dispersive high transparent toothpaste silica of the present invention and preparation method thereof
The polyethylene glycol that molecular weight is 4000, polyethylene glycol are added in S1, the sodium silicate solution for being 2.0mol/L to concentration
Additional amount be sodium silicate solution 8wt%, be dispersed with stirring uniformly, obtain sodium metasilicate mixed solution;
S2, the metabisulfite solution 11m that mass percent concentration is 5.0% is added into reactor tank3, setting stirring unit frequency
For 35Hz, stirring is opened, is warming up to 75 DEG C;
S3, stirring is lower while sodium metasilicate mixed solution 8m is added3It is carried out in cocurrent with concentration for the sulfuric acid solution of 10mol/L
And reaction, the flow velocity of control sodium metasilicate mixed solution are 14m3/ h, sulfuric acid solution flow velocity be 3.0m3/ h, reaction process pH value are
9.5, reaction temperature be 75 DEG C, when sodium metasilicate mixed solution be added after, continue be added dropwise sulfuric acid solution, when pH value be 5.0, stop
Only acid adding obtains silica;
S4, obtained silica is carried out to filters pressing, washing, by obtaining low partial size high dispersive after spray drying treatment
High transparent toothpaste silica.
Comparative example 1
Compared with Example 3, the difference of this comparative example is only that: the molecular weight of polyethylene glycol is 2000.
Comparative example 2
Compared with Example 3, the difference of this comparative example is only that: the molecular weight of polyethylene glycol is 8000.
Comparative example 3
Compared with Example 3, the difference of this comparative example is only that: it is sodium silicate solution that polyethylene glycol, which adds weight,
9wt%.
Comparative example 4
Compared with Example 3, the difference of this comparative example is only that: it is sodium silicate solution that polyethylene glycol, which adds weight,
3wt%.
Comparative example 5
Compared with Example 3, the difference of this comparative example is only that: not using polyethylene glycol as reaction promoter.Specific mistake
Journey is as follows:
S1, the metabisulfite solution 10m that mass percent concentration is 4.5% is added into reactor tank3, setting stirring unit frequency
For 30Hz, stirring is opened, is warming up to 75 DEG C;
S2, stirring is lower while the sodium silicate solution 10m that concentration is 2.2mol/L is added3The sulfuric acid for being 8mol/L with concentration
Solution carries out cocurrent neutralization reaction, and the flow velocity for controlling sodium silicate solution is 14m3/ h, sulfuric acid solution flow velocity be 3.5m3/ h, reaction
Process pH value is 9.0, and reaction temperature is 75 DEG C, after sodium silicate solution is added, continues that sulfuric acid solution is added dropwise, when pH value is
4.8, stop acid adding, obtains silica;
S3, obtained silica is carried out to filters pressing, washing, by obtaining silica after spray drying treatment.
The performance detection of test example one, the low partial size high dispersive high transparent toothpaste silica of the present invention
Each 5g of silica made from the embodiment of the present invention 1~4, comparative example 1~5 is taken, is scattered in 95g mass point respectively
Number is in 70% sorbitol solution, after being sufficiently stirred, standing observes the dispersion of silica sample;Then,
Using the light transmittance (test of the sorbitol solution system light transmittance and each solution system of visible spectrophotometer test 70%
Range 0%~99.9%);Finally, using the size distribution of laser diffractometry (GB/T 19077.1-2008) measurement silica
(particle diameter distribution/μm).Testing result is as shown in table 1 below.
The performance test results of each silica of table 1
From upper table 1:
(1) particle diameter distribution of 1~4 silica of the embodiment of the present invention is 8~15 μm, is scattered in sorbitol solution, point
Function admirable is dissipated, can get uniform, soilless sticking system, it is right by visible spectrophotometer test system light transmittance >=93%
The light transmittance of 70% sorbitol solution has no significant effect.
(2) compared with the embodiment of the present invention 3, comparative example 1,3,4 changes the molecular weight that parameter is respectively polyethylene glycol and is
2000, the 3wt% that polyethylene glycol addition weight is the 9wt% of sodium silicate solution, polyethylene glycol addition weight is sodium silicate solution,
Corresponding obtained silica particle diameter distribution is more than 15 μm, and particle diameter distribution is inhomogenous, and solution system is easy to appear reunion
Object;It is 8000 that comparative example 2, which changes the molecular weight that parameter is polyethylene glycol, and silica particle diameter distribution obtained is obviously too small, inspection
The light transmittance for surveying comparative example 1~4 is below 90%.
(3) compared with the embodiment of the present invention 3, comparative example 5 does not add polyethylene glycol as reaction promoter, obtained dioxy
The light transmittance of SiClx can exceed that 90%, occur bulk aggregate in solution system at this time, and only suspend a small amount of titanium dioxide in solution
Silicon, high transparency is primarily due to the influence of sorbierite light transmittance, and the particle diameter distribution of aggregate is 38~46 μm, leads to the later period
It needs to carry out Particle Breakage processing, can just be satisfied in toothpaste production, the increased costs of investment.
Prompt in the present invention, does reaction promoter with the polyethylene glycol of suitable molecular weight and additive amount, can prevent titanium dioxide
Reunite between silicon particle, improve system uniformity, and makes silica that there is high transparency and low partial size silica etc.
Characteristic meets toothpaste production and requires.
The application effect of test example two, the low partial size high dispersive high transparent toothpaste silica of the present invention
The low partial size high dispersive high transparent toothpaste of the embodiment of the present invention 1~4 silica is applied in toothpaste, respectively
Toothpaste 1~4 is made.
The specific formula of toothpaste 1~4 is following (mass percent): embodiment silica 20%, sorbierite 62%, poly- second
Glycol 8%, hydroxyethyl cellulose 0.6%, guar gum 0.4%, saccharin sodium 0.2%, sodium benzoate 0.2%, sodium lauryl sulfate
2% and water 6.6%.
The specific formula of ordinary toothpaste is following (mass percent): 5 silica 20% of comparative example, gathers sorbierite 62%
Ethylene glycol 8%, hydroxyethyl cellulose 0.6%, guar gum 0.4%, saccharin sodium 0.2%, sodium benzoate 0.2%, lauryl alcohol sulfuric acid
Sodium 2% and water 6.6%.
Above-mentioned toothpaste is detected by 8372 toothpaste standard of GB/T, lotion appearance children is sliding fine and smooth, glittering and translucent, transparent
Degree is high, and pH value 7.4, consistency is moderate, is 14mm, predominantly detects the requirement that index result meets toothpaste standard.Wherein, each tooth
The transparency of cream is retested after six months by above-mentioned method as shown in following table 2-1, the transparency of each toothpaste such as following table 2-
Shown in 2.
Each gel toothpaste clarity testing result of table 2-1
Each gel toothpaste clarity testing result (being retested after six months) of table 2-2
From table 2-1 and 2-2:
With the passage of storage time, ordinary toothpaste is due to reuniting silica surface hydroxyl activity height, particle
Apparent activation energy is high, bad dispersibility, reunites in toothpaste to together, and toothpaste slowly becomes dull opaque, after storage six months,
Transparency is decreased obviously, to affect the beauty of toothpaste.And the silica of technique production is due to dispersibility through the invention
Energy is good, transparency is high, and the appearance of manufactured toothpaste is than normal transparent toothpaste light, and after storage six months, toothpaste appearance remains unchanged
Keep the high grade of transparency.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (9)
1. a kind of preparation method of low partial size high dispersive high transparent toothpaste silica, which comprises the following steps:
S1, polyethylene glycol is added into sodium silicate solution, is dispersed with stirring uniformly, obtains sodium metasilicate mixed solution;
S2,10~12m of metabisulfite solution is added into reactor tank3, stirring is opened, is warming up to 70~75 DEG C;
S3, stirring is lower while 8~10m of sodium metasilicate mixed solution is added dropwise3And sulfuric acid solution, control the flow velocity of sodium metasilicate mixed solution
For 13~14m3/ h, reaction process pH value are 8.5~9.5, and reaction temperature is 70~75 DEG C, when sodium metasilicate mixed solution has been added
Bi Hou continues that sulfuric acid solution is added dropwise, and when pH is 4.0~5.0, stops acid adding, obtains silica;
S4, silica is carried out to filters pressing, washing, by obtaining low partial size high dispersive high transparent toothpaste after spray drying treatment
Use silica.
2. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the concentration of the sodium silicate solution is 2.0~3.5mol/L.
3. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the molecular weight of the polyethylene glycol is 4000~6000.
4. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the additional amount of the polyethylene glycol is 4~8wt% of sodium silicate solution.
5. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the mass percent concentration of the metabisulfite solution is 4.0~6.0%.
6. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the concentration of the sulfuric acid solution is 8~10mol/L.
7. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the flow velocity of the sulfuric acid solution is 2.5~3.5m3/h。
8. the preparation method of low partial size high dispersive high transparent toothpaste silica according to claim 1, feature exist
In the frequency of the stirring is 25~35Hz.
9. the preparation method of described in any item low partial size high dispersive high transparent toothpaste silica according to claim 1~8
Obtained silica.
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CN113023736A (en) * | 2021-04-01 | 2021-06-25 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide for high-oil-absorption low-viscosity toothpaste |
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CN112938994A (en) * | 2021-03-23 | 2021-06-11 | 广州市飞雪材料科技有限公司 | Sand-feeling silica for toothpaste and preparation method thereof |
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CN113307278B (en) * | 2021-06-02 | 2022-01-18 | 广州市飞雪材料科技有限公司 | High-cleaning-performance high-viscosity friction type silicon dioxide and preparation method thereof |
CN114538452A (en) * | 2022-03-15 | 2022-05-27 | 金三江(肇庆)硅材料股份有限公司 | Silica wet gel with narrow particle size distribution and preparation method and application thereof |
CN115571888A (en) * | 2022-10-14 | 2023-01-06 | 福建正盛无机材料股份有限公司 | Preparation method of silicon dioxide for PE separator of storage battery |
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