CN105776230B - Preparation method of silicon dioxide for transparent tooth cleaning toothpaste - Google Patents
Preparation method of silicon dioxide for transparent tooth cleaning toothpaste Download PDFInfo
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- CN105776230B CN105776230B CN201610111901.7A CN201610111901A CN105776230B CN 105776230 B CN105776230 B CN 105776230B CN 201610111901 A CN201610111901 A CN 201610111901A CN 105776230 B CN105776230 B CN 105776230B
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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
- 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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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention belongs to the technical field of silicon dioxide for toothpaste, and relates to a preparation method of silicon dioxide for transparent tooth cleaning toothpaste.The preparation method comprises the steps that 1, a sodium carbonate solution is prepared and added into a sodium silicate solution to obtain a mixed solution; 2, a sodium sulfate solution is added into a reaction kettle, the sodium silicate solution and a sulfuric acid solution are simultaneously and dropwise added while stirring under heating is performed, the process pH is kept to be 7.5-9.5, the end point pH is controlled to be 6.0-7.0, and stirring is performed; 3, water is added, the mixed solution and the sulfuric acid solution are simultaneously and dropwise added while stirring under heating is performed, the process pH is kept to be 5.5-7.5, the reaction end point pH is controlled to be 6.0-7.0, and stirring, filter pressing, washing, drying and crushing are performed to obtain the silicon dioxide.According to silicon dioxide, the copper loss value is 12-15 mg, the light transmittance reaches up to 98%, the oil absorption value is 130-160 ml/100 g, the water absorption capacity is 26-32 ml/20 g, and silicon dioxide is suitable for the transparent tooth cleaning toothpaste.
Description
Technical field
The invention belongs to Silica Using for Toothpaste technical field, and in particular to a kind of transparent toothpaste silicon dioxide that cleans the teeth
Preparation method.
Background technology
In recent years, transparent toothpaste is increasingly favored by people, especially the transparent type toothpaste of high friction spatter property, its
Both there is glittering and translucent, bright in colour outward appearance, and had there is tooth-whitening.
At present, silicon dioxide is spherical loose structure, does not have the abrasion tooth that sharp corner angle will not be excessive, and has
Physicochemical properties are stable, cleaning capacity is strong, and toothpaste Miscibility it is good, the features such as the preparation of transparent toothpaste can be used for, mesh
It is front to be widely used in toothpaste industry.But generally, the high silicon dioxide friction of light transmittance is worth low, cleaning effect
It is not good, and the silicon dioxide light transmittance of high friction value is relatively low, it is impossible to apply well, even if while there is high transmission rate（Printing opacity
Rate is more than 90%）With high friction（Copper loss value is more than 10mg）, but its thickening effect is not good, still needs to and thickening type silicon dioxide
Compounding use, this is designed to formulation of tooth-paste, manufacture and bring some inconvenience, and in formulation of tooth-paste water content than relatively low,
Relative cost can increase.
RDA value is to generally acknowledge the important Testing index for weighing silicon dioxide attriting performance size.As the measure of RDA value is operated
More complicated, requirement of experiment is higher, and almost also no testing agency domestic at present determines RDA value.Compared with RDA value, copper
The measure of consumption value is more convenient, and operability is higher, and there is certain positive relationship between RDA value and copper loss value.Typically
For, the copper loss value of general silica is within 2.0mg；The copper loss value of medium friction type silicon dioxide 2.0 ~ 10.0mg it
Between；The copper loss value of high friction type silicon dioxide is then more than 10.0mg, is usually no more than 20.0mg and is advisable, dentium nitor otherwise easy to wear
Matter.And the light transmittance of silicon dioxide have to be larger than 90%, transparent type transparent toothpaste can be just prepared.
105236415 A of Chinese patent application CN discloses a kind of preparation method of core-shell sediment silica, the party
Method takes two step hydrothermal depositions to react mainly with sodium silicate and sulphuric acid as raw material, the material concentration, reaction in control course of reaction
The process conditions such as the temperature of system and pH value, prepare with core-shell sediment silica.The RDA of the precipitated silica
It is 54ml/20gH to be worth and be more than or equal to 100, water absorption for 196, PCR value2O, with excellent wear-resisting clean-up performance and water suction
Amount, but the precipitated silica light transmittance is relatively low, is not particularly suited in transparent toothpaste.Chinese patent application CN 103274422
A also discloses that a kind of method for preparing core-shell sediment silica, likewise, silicon dioxide obtained in the method have it is excellent
Wear-resisting clean-up performance and water absorption, but its light transmittance is still relatively low, is not suitable for transparent toothpaste.
In sum, it is necessary to research and develop one kind and prepare high friction spatter property, high transmission rate, and with the saturating of thickening power
The method of bright Silica Using for Toothpaste.
The content of the invention
In order to solve problems of the prior art, it is an object of the invention to provide one kind cleans the teeth, transparent toothpaste uses two
The preparation method of silicon oxide, improvement of the method by technique so that silicon dioxide is while keeping higher removal to wipe spatter property
With very high light transmittance, and there is thickening power.
To achieve these goals, technical scheme is as follows：
A kind of preparation method of the transparent toothpaste silicon dioxide that cleans the teeth, comprises the following steps：
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3 ~ 3.45, the modulation concentration respectively that adds water is
2.5 ~ 3.2M sodium silicate solutions and concentration are 1.6 ~ 2.2M sodium silicate solutions, standby；
Configuration concentration expressed in percentage by weight is 25 ~ 28% sodium carbonate liquor, is then added into the silicic acid that concentration is 1.6 ~ 2.2M
In sodium solution, stir, obtain mixed liquor, it is standby；
Second step：4 ~ 8m is added toward reactor3Concentration expressed in percentage by weight is 11.0 ~ 15.0% metabisulfite solution, is heated to
70 ~ 80 DEG C, the lower Deca concentration simultaneously of stirring is 2.5 ~ 3.2M, 3 ~ 5m of sodium silicate solution3It is molten for the sulphuric acid of 10.0 ~ 12.0M with concentration
Liquid, keeps process pH to be 7.5 ~ 9.5, and after sodium silicate solution completion of dropping, it is 6.0 ~ 7.0 to continue Deca sulfuric acid solution to pH, is stopped
Only acid adding, stirs 10 ~ 15min；
3rd step：4 ~ 6m is continuously added toward aforesaid reaction vessel3Water, be heated to 70 ~ 80 DEG C, the lower Deca institute simultaneously of stirring
State 8 ~ 10m of mixed liquor3It is the sulfuric acid solution of 10.0 ~ 12.0M with concentration, keeps process pH to be 5.5 ~ 7.5, mixed liquor completion of dropping
Afterwards, it is 6.0 ~ 7.0 to control reaction end pH, stops acid adding, stirs 10 ~ 15min, and gas is used in filter pressing, washing after spray drying
Stream crusher in crushing is 7 ~ 15 μm to particle diameter, obtains silicon dioxide.
Further, in the mixed liquor, the weight content of sodium carbonate is 0.2 ~ 1%.
Further, in the mixed liquor, the weight content of sodium carbonate is 0.6%.
Further, the speed for stirring in the second step, the 3rd step is 35Hz.
Further, in the second step, the rate of addition of sodium silicate solution is 15m3/h。
In the preparation method that the present invention cleans the teeth transparent toothpaste silicon dioxide, using two step hydrothermal deposition methods, the first step,
Using the sodium sulfate that concentration expressed in percentage by weight is 11.0 ~ 15.0% as reaction promoter, added at a high temperature of 70 ~ 80 DEG C simultaneously dense
It is that 2.5 ~ 3.2M sodium silicate solutions and concentration carry out soda acid with dripping for the sulphuric acid of 10.0 ~ 12.0M to spend, and control second step is quickly anti-
Should, the time is 10 ~ 20min, and keeps process pH to be 7.5 ~ 9.5, and terminal pH is 6.0 ~ 7.0, and transparent fine and close core knot is obtained
Structure, then second step is using water as bottom liquid, adds the sodium silicate solution containing sodium carbonate equally at a high temperature of 70 ~ 80 DEG C simultaneously
With concentration for 10.0 ~ 12.0M sulfuric acid solution carry out soda acid with drip, and control process pH be 5.5 ~ 7.5, terminal pH be 6.0 ~
7.0, transparent loose shell structure is obtained, sodium carbonate discharges bubble in the reaction so that shell structure is more loose, so as to ensure system
The existing high friction cleaning value of silicon dioxide for obtaining and light transmittance, have thickening power again.
Therefore, compared with prior art, advantage of the invention is that：
（1）The present invention clean the teeth transparent toothpaste silicon dioxide preparation method obtained in silicon dioxide copper loss value be 12 ~
15mg, light transmittance are more than 95%, reach as high as 98%, and oil factor is 130 ~ 160ml/100g, 26 ~ 32ml/20g of water absorption, and fluorine
Compatibility ＞ 90%, with friction spatter property and the high grade of transparency well, and has thickening power.
（2）The present invention clean the teeth transparent toothpaste silicon dioxide preparation method obtained in silicon dioxide be applied to transparent toothpaste
In, addition is 15 ~ 20%, that is, can have cleaning effect well separately as abrasive without the need for compounding with thickening type silicon dioxide
In fruit and thickening effect, and toothpaste, water consumption increases, and 16 ~ 21%, toothpaste is still glittering and translucent, and the transparency very well, is significantly reduced
The production cost of toothpaste.
（2）The present invention clean the teeth transparent toothpaste silicon dioxide preparation method it is simple to operate, condition is controllable, process stabilizing,
Can industrialized production, be conducive to popularization and application.
Specific embodiment
Describe the present invention, the illustrative examples of the here present invention and explanation below in conjunction with specific embodiment in detail
It is for explaining the present invention but not as a limitation of the invention.
In the present invention, RDA value is according to Determination of the Relative Dentin Abrasion Level
of
The method of Powder is tested；Copper loss value and light transmittance are according to existing general method（Such as Wang Xianwei etc. is delivered
Entitled " development and its application in toothpaste of high friction transparent type silicon dioxide " on oral care implement industry magazine
Paper in correlation method）Tested；Water absorption and oil factor are according to industry standard QB/T2346 Silica Using for Toothpaste
Standard testing；The fluorine compatibility is tested according to Fluoride ion selective electrode method.
The preparation method of embodiment 1, the transparent toothpaste silicon dioxide that cleans the teeth of the invention
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3 ~ 3.45, the modulation concentration respectively that adds water is
2.5M sodium silicate solutions and concentration are 1.6M sodium silicate solutions, standby；
Configuration concentration expressed in percentage by weight is 25% sodium carbonate liquor, is then added into the sodium silicate solution that concentration is 1.6M
In, stirring, obtain mixed liquor, in mixed liquor, the weight content of sodium carbonate is 0.2%, standby；
Second step：4m is added toward reactor3Concentration expressed in percentage by weight is 11.0% metabisulfite solution, is heated to 80 DEG C, stirs
It is 2.5M sodium silicate solution 3m to mix down Deca concentration simultaneously3It is the sulfuric acid solution of 10.0M with concentration, keeps process pH to be 7.5, silicon
The rate of addition of acid sodium solution is 15m3/ h, after sodium silicate solution completion of dropping, it is 6.0 to continue Deca sulfuric acid solution to pH, is stopped
Only acid adding, stirs 10min；
3rd step：4m is continuously added toward aforesaid reaction vessel3Water, be heated to 80 DEG C, mix described in the lower Deca simultaneously of stirring
Close liquid 10m3It is the sulfuric acid solution of 10.0M with concentration, keeps process pH to be 5.5, after mixed liquor completion of dropping, control reaction end
PH is 6.0, stops acid adding, stirs 10min, and filter pressing, washing use airflow crash crusher machine to particle diameter to be 10 after spray drying
μm, obtain silicon dioxide.
The speed stirred in the second step, the 3rd step is 35Hz.
After testing, the copper loss value of obtained silicon dioxide is 12mg, and light transmittance is 96%, and oil factor is 160ml/100g, is inhaled
The water yield is 32ml/20g, and the fluorine compatibility is 95%.
The preparation method of embodiment 2, the transparent toothpaste silicon dioxide that cleans the teeth of the invention
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3 ~ 3.45, the modulation concentration respectively that adds water is
3.2M sodium silicate solutions and concentration are 2.2M sodium silicate solutions, standby；
Configuration concentration expressed in percentage by weight is 28% sodium carbonate liquor, is then added into the sodium silicate solution that concentration is 2.2M
In, stirring, obtain mixed liquor, in mixed liquor, the weight content of sodium carbonate is 1%, standby；
Second step：8m is added toward reactor3Concentration expressed in percentage by weight is 15.0% metabisulfite solution, is heated to 70 DEG C, stirs
It is 3.2M sodium silicate solution 5m to mix down Deca concentration simultaneously3It is the sulfuric acid solution of 12.0M with concentration, keeps process pH to be 9.5, silicon
The rate of addition of acid sodium solution is 15m3/ h, after sodium silicate solution completion of dropping, it is 7.0 to continue Deca sulfuric acid solution to pH, is stopped
Only acid adding, stirs 15min；
3rd step：6m is continuously added toward aforesaid reaction vessel3Water, be heated to 70 DEG C, mix described in the lower Deca simultaneously of stirring
Close liquid 8m3It is the sulfuric acid solution of 12.0M with concentration, keeps process pH to be 7.5, after mixed liquor completion of dropping, control reaction end
PH is 7.0, stops acid adding, stirs 15min, and filter pressing, washing use airflow crash crusher machine to particle diameter to be 10 after spray drying
μm, obtain silicon dioxide.
The speed stirred in the second step, the 3rd step is 35Hz.
After testing, the copper loss value of obtained silicon dioxide is 15mg, and light transmittance is 95%, and oil factor is 130ml/100g, is inhaled
The water yield is 28ml/20g, and the fluorine compatibility is 96%.
The preparation method of embodiment 3, the transparent toothpaste silicon dioxide that cleans the teeth of the invention
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3 ~ 3.45, the modulation concentration respectively that adds water is
2.8M sodium silicate solutions and concentration are 2.0M sodium silicate solutions, standby；
Configuration concentration expressed in percentage by weight is 26% sodium carbonate liquor, is then added into the sodium silicate solution that concentration is 2.0M
In, stirring, obtain mixed liquor, in mixed liquor, the weight content of sodium carbonate is 0.6%, standby；
Second step：6m is added toward reactor3Concentration expressed in percentage by weight is 13.0% metabisulfite solution, is heated to 75 DEG C, stirs
It is 2.8M sodium silicate solution 4m to mix down Deca concentration simultaneously3It is the sulfuric acid solution of 10.0M with concentration, keeps process pH to be 8.5, silicon
The rate of addition of acid sodium solution is 15m3/ h, after sodium silicate solution completion of dropping, it is 7.0 to continue Deca sulfuric acid solution to pH, is stopped
Only acid adding, stirs 10min；
3rd step：5m is continuously added toward aforesaid reaction vessel3Water, be heated to 75 DEG C, mix described in the lower Deca simultaneously of stirring
Close liquid 9m3It is the sulfuric acid solution of 10.0M with concentration, keeps process pH to be 6.5, after mixed liquor completion of dropping, control reaction end
PH is 7.0, stops acid adding, stirs 10min, and filter pressing, washing use airflow crash crusher machine to particle diameter to be 10 after spray drying
μm, obtain silicon dioxide.
The speed stirred in the second step, the 3rd step is 35Hz.
After testing, the copper loss value of obtained silicon dioxide is 14mg, and light transmittance is 98%, and oil factor is 160ml/100g, is inhaled
The water yield is 32ml/20g, and the fluorine compatibility is 96%.
The preparation method of embodiment 4, the transparent toothpaste silicon dioxide that cleans the teeth of the invention
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3 ~ 3.45, the modulation concentration respectively that adds water is
3.0M sodium silicate solutions and concentration are 1.8M sodium silicate solutions, standby；
Configuration concentration expressed in percentage by weight is 25% sodium carbonate liquor, is then added into the sodium silicate solution that concentration is 1.8M
In, stirring, obtain mixed liquor, in mixed liquor, the weight content of sodium carbonate is 0.4%, standby；
Second step：8m is added toward reactor3Concentration expressed in percentage by weight is 15.0% metabisulfite solution, is heated to 80 DEG C, stirs
It is 3.0M sodium silicate solution 5m to mix down Deca concentration simultaneously3It is the sulfuric acid solution of 11.0M with concentration, keeps process pH to be 9.5, silicon
The rate of addition of acid sodium solution is 15m3/ h, after sodium silicate solution completion of dropping, it is 7.0 to continue Deca sulfuric acid solution to pH, is stopped
Only acid adding, stirs 10min；
3rd step：4m is continuously added toward aforesaid reaction vessel3Water, be heated to 80 DEG C, mix described in the lower Deca simultaneously of stirring
Close liquid 9m3It is the sulfuric acid solution of 11.0M with concentration, keeps process pH to be 7.0, after mixed liquor completion of dropping, control reaction end
PH is 6.0, stops acid adding, stirs 10min, and filter pressing, washing use airflow crash crusher machine to particle diameter to be 10 after spray drying
μm, obtain silicon dioxide.
The speed stirred in the second step, the 3rd step is 35Hz.
After testing, the copper loss value of obtained silicon dioxide is 13mg, and light transmittance is 96%, and oil factor is 150ml/100g, is inhaled
The water yield is 30ml/20g, and the fluorine compatibility is 94%.
Comparative example one,
Embodiment 4 in 103274422 A of Chinese patent application CN.After testing, the copper loss of obtained silicon dioxide
It is worth for 19mg, light transmittance is 73%, oil factor is 100ml/100g, and water absorption is 34ml/20g, and the fluorine compatibility is 95%.
Comparative example two,
Embodiment two in 105236415 A of Chinese patent application CN.After testing, the copper of obtained silicon dioxide
Consumption value is 15mg, and light transmittance is 82%, and oil factor is 120ml/100g, and water absorption is 54ml/20g, and the fluorine compatibility is 95%.
Comparative example three,
Compared with Example 3, the difference of this comparative example is：3rd step：5m is continuously added toward aforesaid reaction vessel3's
Water, is heated to 75 DEG C, adds concentration for the sulfuric acid solution of 10.0M（About 2m3）, stirring, the addition mixed liquor 9m3, when reaction knot
Shu Shi, the pH of reaction system is 7.0, stirs 10min, and filter pressing, washing use airflow crash crusher machine after spray drying to grain
Footpath is 10 μm, obtains silicon dioxide.
Other operations and parameter are with embodiment 3.
After testing, the copper loss value of obtained silicon dioxide is 4mg, and light transmittance is 64%, and oil factor is 160ml/100g, is inhaled
The water yield is 35ml/20g, and the fluorine compatibility is 92%.
Comparative example four,
Compared with Example 3, the difference of this comparative example is that this comparative example does not use sodium carbonate, is comprised the following steps that：
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3 ~ 3.45, the modulation concentration respectively that adds water is
2.8M sodium silicate solutions and concentration are 2.0M sodium silicate solutions, standby；
Second step：6m is added toward reactor3Concentration expressed in percentage by weight is 13.0% metabisulfite solution, is heated to 75 DEG C, stirs
It is 2.8M sodium silicate solution 4m to mix down Deca concentration simultaneously3It is the sulfuric acid solution of 10.0M with concentration, keeps process pH to be 8.5, silicon
The rate of addition of acid sodium solution is 15m3/ h, after sodium silicate solution completion of dropping, it is 7.0 to continue Deca sulfuric acid solution to pH, is stopped
Only acid adding, stirs 10min；
3rd step：5m is continuously added toward aforesaid reaction vessel3Water, be heated to 75 DEG C, the lower Deca concentration simultaneously of stirring is
2.0M sodium silicate solution 9m3It is the sulfuric acid solution of 10.0M with concentration, keeps process pH to be 6.5, after mixed liquor completion of dropping, control
Reaction end pH processed is 7.0, stops acid adding, stirs 10min, and airflow crash crusher machine is used in filter pressing, washing after spray drying
It is 10 μm to particle diameter, obtains silicon dioxide.
The speed stirred in the second step, the 3rd step is 35Hz.
After testing, the copper loss value of obtained silicon dioxide is 19mg, and light transmittance is 76%, and oil factor is 90ml/100g, is inhaled
The water yield is 26ml/20g, and the fluorine compatibility is 94%.
Comparative example five,
Compared with Example 3, the difference of this comparative example is：In the mixed liquor, the weight content of sodium carbonate is 2%
Other operations and parameter are with embodiment 3.
After testing, the copper loss value of obtained silicon dioxide is 6mg, and light transmittance is 82%, and oil factor is 150ml/100g, is inhaled
The water yield is 30ml/20g, and the fluorine compatibility is 91%.
Comparative example six,
Compared with Example 3, the difference of this comparative example is：The pH for controlling second step and three-step reaction terminal is 4.0.
Other operations and parameter are with embodiment 3.
After testing, the copper loss value of obtained silicon dioxide is 7mg, and light transmittance is 86%, and oil factor is 130ml/100g, is inhaled
The water yield is 30ml/20g, and the fluorine compatibility is 90%.
Comparative example seven,
Compared with Example 3, the difference of this comparative example is：Sulphuric acid of the concentration for 6.0M used in second step and the 3rd step
Solution.
Other operations and parameter are with embodiment 3.
After testing, the copper loss value of obtained silicon dioxide is 9mg, and light transmittance is 85%, and oil factor is 120ml/100g, is inhaled
The water yield is 35ml/20g, and the fluorine compatibility is 93%.
Comparative example eight,
Compared with Example 3, the difference of this comparative example is：In second step and the 3rd step, the temperature of course of reaction is 65
℃。
Other operations and parameter are with embodiment 3.
After testing, the copper loss value of obtained silicon dioxide is 5mg, and light transmittance is 90%, and oil factor is 100ml/100g, is inhaled
The water yield is 24ml/20g, and the fluorine compatibility is 94%.
To sum up, 1 ~ 4 present invention of the embodiment of the present invention clean the teeth transparent toothpaste silicon dioxide preparation method obtained in dioxy
SiClx has high friction cleaning, the characteristic of high transmission rate, and has thickening power, and its copper loss value is 12 ~ 15mg, and light transmittance is big
In 95%, 98% is reached as high as, oil factor is 130 ~ 160ml/100g, 26 ~ 32ml/20g of water absorption, and fluorine compatibility ＞ 90%, tool
There is good compatibility, in the good dispersion of toothpaste system, it is adaptable to all types of toothpaste, be particularly suited for abrasive transparent type tooth
Cream.
Silicon dioxide obtained in the embodiment of the present invention 3 is applied in toothpaste, Ju Ti Pei Fang is as follows（According to percentage by weight
Meter）：Sorbitol 60%, water 18%, surfactant 2.3%, binding agent 0.9%, essence 0.8%, silica 1 8%, obtained toothpaste
Transparency is high；Compared to the formula of existing transparent toothpaste（The water yield is 10 ~ 11%）, and used two obtained in the embodiment of the present invention 3
After silicon oxide, the water yield increases, and 16 ~ 21%, the total amount reduction of Sorbitol and silicon dioxide, toothpaste are still transparent, significantly reduce
The production cost of toothpaste.
In technical solution of the present invention, the 3rd step is fed by the way of alkali drop acid（Comparative example three）, which is obtained obtained
Silicon dioxide is hard gel, and copper loss value and light transmittance decline, it is impossible to reach high friction, the purpose of high transparency；Do not make in reaction
Use sodium carbonate（Comparative example four）So that the structure of silicon dioxide is excessively fine and close, causes that copper loss value is excessive, and light transmittance also declines, and
Using excessive sodium carbonate（Comparative example five）Then so that the structure of silicon dioxide is excessively loose, copper loss value does not reach requirement；Reaction
PH value（Comparative example six）, material concentration（Comparative example seven）And reaction temperature（Comparative example eight）The property of silicon dioxide can be produced
It is raw to affect, and these affect that number is irregular can be target-seeking, illustrate that the preparation method of the transparent toothpaste silicon dioxide that cleans the teeth of the invention is each
Complement each other between step.
The principle and its effect of above-described embodiment only illustrative present invention, it is of the invention not for limiting.It is any ripe
The personage for knowing this technology all can carry out modifications and changes to above-described embodiment under the spirit and the scope without prejudice to the present invention.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (4)
1. a kind of preparation method of the transparent toothpaste silicon dioxide that cleans the teeth, it is characterised in that comprise the following steps：
The first step：By SiO2:Na2After the sodium silicate solid High-temperature Liquefaction of O=3.3～3.45, add water
～3.2M sodium silicate solutions and concentration are 1.6～2.2M sodium silicate solutions, standby；
Configuration concentration expressed in percentage by weight is 25～28% sodium carbonate liquor, is then added into the silicic acid that concentration is 1.6～2.2M
In sodium solution, stir, obtain mixed liquor, it is standby；In the mixed liquor, the weight content of sodium carbonate is 0.2～1%；
Second step：4～8m is added toward reactor3Concentration expressed in percentage by weight is 11.0～15.0% metabisulfite solution, is heated to 70
～80 DEG C, the lower Deca concentration simultaneously of stirring is 2.5～3.2M, 3～5m of sodium silicate solution3With the sulphuric acid that concentration is 10.0～12.0M
Solution, keep process pH be 7.5～9.5, after sodium silicate solution completion of dropping, continue Deca sulfuric acid solution to pH be 6.0～
7.0, stop acid adding, stir 10～15min；
3rd step：4～6m is continuously added toward aforesaid reaction vessel3Water, be heated to 70～80 DEG C, described in the lower Deca simultaneously of stirring
8～10m of mixed liquor3With the sulfuric acid solution that concentration is 10.0～12.0M, process pH is kept to be 5.5～7.5, mixed liquor is dripped
Bi Hou, it is 6.0～7.0 to control reaction end pH, stops acid adding, stirs 10～15min, and filter pressing is washed, after spray drying
It is 7～15 μm with airflow crash crusher machine to particle diameter, obtains silicon dioxide.
2. clean the teeth the preparation method of transparent toothpaste silicon dioxide as claimed in claim 1, it is characterised in that in the mixed liquor
The weight content of sodium carbonate is 0.6%.
3. clean the teeth the preparation method of transparent toothpaste silicon dioxide as claimed in claim 1, it is characterised in that the second step,
The speed stirred in 3rd step is 35Hz.
4. clean the teeth the preparation method of transparent toothpaste silicon dioxide as claimed in claim 1, it is characterised in that in the second step
The rate of addition of sodium silicate solution is 15m3/h。
Priority Applications (1)
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| CN106276929B (en) * | 2016-07-29 | 2017-07-07 | 广州市飞雪材料科技有限公司 | A kind of preparation method of friction type silica |
| CN107739035B (en) * | 2017-09-28 | 2018-07-13 | 广州市飞雪材料科技有限公司 | A kind of coloring stabilized colored silicon dioxide granule and preparation method thereof |
| CN109607555B (en) * | 2019-01-02 | 2019-08-09 | 广州市飞雪材料科技有限公司 | A kind of high friction high transparent toothpaste silica and preparation method thereof |
| CN109485054B (en) * | 2019-01-02 | 2019-10-01 | 广州市飞雪材料科技有限公司 | A kind of low oil factor high-specific surface area friction type silica and preparation method thereof |
| CN116692884B (en) * | 2023-06-13 | 2024-01-16 | 金三江(肇庆)硅材料股份有限公司 | Silica microsphere with low oil absorption value and high viscosity as well as preparation method and application thereof |
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| CN102388124A (en) * | 2009-04-06 | 2012-03-21 | 昂里克·埃尔南德斯 | Silicas and alkali metal salt compositions, detergents formed from such compositions and method of forming such composition |
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| CN1221393A (en) * | 1996-06-06 | 1999-06-30 | 罗狄亚化学公司 | Silica capable of being used in toothpaste composition |
| CN1225074A (en) * | 1996-07-05 | 1999-08-04 | 罗狄亚化学公司 | Abrasive silica to be used in toothpaste |
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