CN105016345B - A kind of preparation method of the colored silicon dioxide granule of toothpaste suspension - Google Patents
A kind of preparation method of the colored silicon dioxide granule of toothpaste suspension Download PDFInfo
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Abstract
The present invention provides the preparation method that a kind of toothpaste suspends colored silicon dioxide granule, comprises the following steps: (1) adds dilute sulfuric acid in retort and stirs, and is simultaneously introduced PEG and sodium dodecyl sulfate aqueous solution;(2) adding water glass solution in retort, be neutralized reaction while stirring, when the pH value of material system reaches 3.0~4.0, add food grade colorant solution, the pH value controlling reaction end is 4.0~5.0;(3) continue to add dilute sulfuric acid in retort, after stirring, add water glass solution, react while stirring and stop after changing into gel to material system adding water glass solution, obtain gel;(4) gel is carried out filter pressing, obtain gel press cake, detergent gel filter cake, remove the PEG of sulfate and residual, gel press cake is dried, pulverizes, obtain silicon dioxide granule.The silicon dioxide granule that the present invention prepares has certain degree of hardness and relative density less, and in toothpaste modulation solution system, suspension time is at least up to half an hour.
Description
Technical field
The preparation method that the present invention relates to the colored silicon dioxide granule of a kind of toothpaste suspension.
Background technology
Colored silicon dioxide granule has the structure of porous and large surface area, physics and stable chemical performance, and color is beautiful, so being widely used in toothpaste, is the very important additive of one of toothpaste.Toothpaste adds silicon dioxide colour particles be possible not only to give the brand-new color of toothpaste and outward appearance, but also possess good clean-up performance, therefore very popular.But, the hardness of the colored silicon dioxide friction particle owing to selling in the market is general higher, relative density is bigger, not past any modifying and decorating, so when modulating toothpaste solution system, the suspension time of colored silicon dioxide granule is too short, is typically within 5min and almost can all be deposited to bottom solution, leverage colored silicon dioxide granule homogeneity in toothpaste and stability, limit the development of this toothpaste.
Such as publication number is CN100345755, publication date is that the Chinese patent of 2007.10.31 discloses " preparation method of a kind of nano silicon ", the method is to be joined by alkali silicate in the mixture of hydrocarbon component, surfactant and cosurfactant, form nanometer titania nanoparticle system of oil bag high concentration alkali metal silicate, make produced nano silicon be limited in micelle and carry out precipitation, it is then passed through washing, dries, obtain nanometer silicon dioxide particle.Silicon dioxide particle size distribution range obtained by this patent is narrow, can be used as toothpaste filler, but its hardness is higher, density is bigger, when modulating toothpaste solution system, suspension time is shorter, is all deposited to bottom solution, scattered homogeneity and less stable in toothpaste system within 5min.
Summary of the invention
The preparation method that the technical problem to be solved in the present invention is to provide the colored silicon dioxide granule of a kind of toothpaste suspension, the silicon dioxide granule prepared has certain degree of hardness and relative density less, in toothpaste modulation solution system, suspension time is at least up to half an hour, it is ensured that it is scattered homogeneity and stability in toothpaste system.
For solving above-mentioned technical problem, the technical scheme is that
The preparation method of the colored silicon dioxide granule of a kind of toothpaste suspension, comprises the following steps:
(1) in retort, add dilute sulfuric acid and stir, it is subsequently adding fully dispersed Aqueous Solutions of Polyethylene Glycol and sodium dodecyl sulfate aqueous solution, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.05~0.1% of dilute sulfuric acid weight, and sodium dodecyl sulfate aqueous solution weight is the 0.05~0.1% of dilute sulfuric acid weight;
(2) adding water glass solution in retort, be neutralized reaction while stirring, when the pH value of material system reaches 3.0~4.0, add food grade colorant solution in retort, the pH value controlling reaction end is 4.0~5.0;
(3) continue to add dilute sulfuric acid in retort, the backward retort that stirs is added water glass solution, be neutralized after reaction changes into gel to material system while stirring and stop adding water glass solution, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove Polyethylene Glycol and the dodecyl sodium sulfate of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the colored silicon dioxide granule of toothpaste suspension.
Wherein, step (2) and in the course of reaction in step (3), the interpolation speed of water glass solution and mixing speed need to strictly control, and so can ensure the stability that silicon dioxide granule structure is formed.
Preferably, in step of the present invention (1), the concentration of dilute sulfuric acid is 0.3~0.4M.
Preferably, in step of the present invention (1), the concentration of Aqueous Solutions of Polyethylene Glycol is 1~10%.
Preferably, in step of the present invention (1), the concentration of sodium dodecyl sulfate aqueous solution is 1~10%.
Preferably, in step of the present invention (2), the modulus of water glass solution is 3.3, and the concentration of water glass solution is 0.3~0.4M.
Preferably, in step of the present invention (2), the interpolation speed of water glass solution is 1500~2000L/h.
Preferably, in step of the present invention (2), food grade colorant solution is the sorbitol of food stage, glycerol or polyglycol solution, and it adds weight is the 0.1~0.5% of dilute sulfuric acid.
Preferably, in step of the present invention (3), the concentration of dilute sulfuric acid is 0.3~0.4M.
Preferably, in step of the present invention (3), the modulus of water glass solution is 3.3, and the concentration of water glass solution is 0.3~0.4M.
Preferably, in step of the present invention (3), the interpolation speed of water glass solution is 1500~2000L/h.
Compared with prior art, the method have the advantages that
PEG and Polyethylene Glycol, it is oligomer or the polymer of oxirane, it is widely used in cosmetics and pigment industry and makes dispersant, sodium lauryl sulphate is to have good emulsifying, foaming, infiltration, the anion surfactant of decontamination and dispersive property, good with the multiple compatibility of nonionic surfactant Polyethylene Glycol, Polyethylene Glycol and sodium lauryl sulphate are added on the structure that can pass through the micelle that silicon dioxide granule is reacted in change in reaction system and form gel, Polyethylene Glycol and silicon dioxide granule combine with hydrogen bond and uniform adsorption is at particle surface, the surface texture making particle changes and effectively disperses;nullSodium lauryl sulphate produces a large amount of bubble in the solution and is effectively combined with silicon dioxide granule,The Zeta potential value of silicon dioxide granule can be significantly improved simultaneously,Therefore aggregation of particles degree and density are effectively reduced,Improve the dispersion stabilization of particle,And two secondary responses of step (2) and step (3) can make aggregation of particles degree enter once reduced,Keep there is certain porosity between particle,Increase the specific surface area of particle,So that the density of silicon dioxide granule diminishes further,In addition,Polyethylene Glycol、Dodecyl sodium sulfate defines between particle a degree of mutually exclusive and more stable after being combined with silicon dioxide granule,Therefore the suspension time that the silicon dioxide granule prepared is modulated in solution system at toothpaste at least can reach half an hour,Suspension effect is fine,Its scattered homogeneity and stability in toothpaste system can be ensured,The colored toothpaste color thus prepared is homogeneous,Stably dispersing;The present invention strictly controls the addition of Polyethylene Glycol and dodecyl sodium sulfate so that silicon dioxide granule can keep moderate hardness, still has good frictional behaviour and clean-up performance.
Detailed description of the invention
Describing the present invention in detail below in conjunction with specific embodiment, illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1
The preparation method of the blue silicon dioxide granule of a kind of toothpaste suspension, comprises the following steps:
(1) in retort, add concentration to be the dilute sulfuric acid of 0.4M and stir, it is subsequently adding Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 5% and concentration is the sodium dodecyl sulfate aqueous solution of 5%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.1% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.1% of dilute sulfuric acid weight;
(2) in retort with the flow of 1600L/h add modulus be 3.3, concentration be 0.4M water glass solution, it is neutralized reaction while stirring, the strict interpolation speed controlling water glass solution and mixing speed, when the pH value of material system reaches 3.0~4.0, Food-grade blue pigment sorbitol solution is added in retort, its weight is the 0.1% of dilute sulfuric acid, and the pH value controlling reaction end is 4.0~5.0;
(3) continuing to add concentration in retort is the dilute sulfuric acid of 0.4M, the backward retort that stirs is added modulus be 3.3, concentration be the water glass solution of 0.4M, it is neutralized after reaction changes into gel to material system while stirring to stop adding water glass solution, the strict interpolation speed controlling water glass solution and mixing speed, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the blue silicon dioxide granule of toothpaste suspension.
Embodiment 2
The preparation method of the green silicon dioxide granule of a kind of toothpaste suspension, comprises the following steps:
(1) in retort, add concentration to be the dilute sulfuric acid of 0.3M and stir, it is subsequently adding Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 10% and concentration is the sodium dodecyl sulfate aqueous solution of 10%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.06% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.06% of dilute sulfuric acid weight;
(2) in retort with the flow of 1500L/h add modulus be 3.3, concentration be 0.4M water glass solution, it is neutralized reaction while stirring, the strict interpolation speed controlling water glass solution and mixing speed, when the pH value of material system reaches 3.0~4.0, food stage green pigment glycerite is added in retort, its weight is the 0.3% of dilute sulfuric acid, and the pH value controlling reaction end is 4.0~5.0;
(3) continuing to add concentration in retort is the dilute sulfuric acid of 0.3M, the backward retort that stirs is added modulus be 3.3, concentration be the water glass solution of 0.4M, it is neutralized after reaction changes into gel to material system while stirring to stop adding water glass solution, the strict interpolation speed controlling water glass solution and mixing speed, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the green silicon dioxide granule of toothpaste suspension.
Embodiment 3
The preparation method of the red silicon dioxide granule of a kind of toothpaste suspension, comprises the following steps:
(1) in retort, add concentration to be the dilute sulfuric acid of 0.4M and stir, it is subsequently adding Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 9% and concentration is the sodium dodecyl sulfate aqueous solution of 9%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.08% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.08% of dilute sulfuric acid weight;
(2) in retort with the flow of 2000L/h add modulus be 3.3, concentration be 0.3M water glass solution, it is neutralized reaction while stirring, the strict interpolation speed controlling water glass solution and mixing speed, when the pH value of material system reaches 3.0~4.0, food stage red pigments polyglycol solution is added in retort, its weight is the 0.2% of dilute sulfuric acid, and the pH value controlling reaction end is 4.0~5.0;
(3) continuing to add concentration in retort is the dilute sulfuric acid of 0.4M, the backward retort that stirs is added modulus be 3.3, concentration be the water glass solution of 0.3M, it is neutralized after reaction changes into gel to material system while stirring to stop adding water glass solution, the strict interpolation speed controlling water glass solution and mixing speed, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the red silicon dioxide granule of toothpaste suspension.
Embodiment 4
The preparation method of a kind of toothpaste suspension white silicon dioxide granule, comprises the following steps:
(1) in retort, add concentration to be the dilute sulfuric acid of 0.3M and stir, it is subsequently adding Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 4% and concentration is the sodium dodecyl sulfate aqueous solution of 4%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.05% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.05% of dilute sulfuric acid weight;
(2) in retort with the flow of 1800L/h add modulus be 3.3, concentration be 0.4M water glass solution, it is neutralized reaction while stirring, the strict interpolation speed controlling water glass solution and mixing speed, when the pH value of material system reaches 3.0~4.0, food grade white pigment sorbitol solution is added in retort, its weight is the 0.5% of dilute sulfuric acid, and the pH value controlling reaction end is 4.0~5.0;
(3) continuing to add concentration in retort is the dilute sulfuric acid of 0.3M, the backward retort that stirs is added modulus be 3.3, concentration be the water glass solution of 0.4M, it is neutralized after reaction changes into gel to material system while stirring to stop adding water glass solution, the strict interpolation speed controlling water glass solution and mixing speed, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains toothpaste suspension white silicon dioxide granule.
Embodiment 5
The preparation method of the blue silicon dioxide granule of a kind of toothpaste suspension, comprises the following steps:
(1) in retort, add concentration to be the dilute sulfuric acid of 0.3M and stir, it is subsequently adding Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 8% and concentration is the sodium dodecyl sulfate aqueous solution of 8%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.09% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.09% of dilute sulfuric acid weight;
(2) in retort with the flow of 1900L/h add modulus be 3.3, concentration be 0.3M water glass solution, it is neutralized reaction while stirring, the strict interpolation speed controlling water glass solution and mixing speed, when the pH value of material system reaches 3.0~4.0, Food-grade blue pigment sorbitol solution is added in retort, its weight is the 0.4% of dilute sulfuric acid, and the pH value controlling reaction end is 4.0~5.0, continuation stirring changes into gel to material system;
(3) continuing to add concentration in retort is the dilute sulfuric acid of 0.3M, the backward retort that stirs is added modulus be 3.3, concentration be the water glass solution of 0.3M, it is neutralized after reaction changes into gel to material system while stirring to stop adding water glass solution, the strict interpolation speed controlling water glass solution and mixing speed, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the blue silicon dioxide granule of toothpaste suspension.
Embodiment 6
The preparation method of the green silicon dioxide granule of a kind of toothpaste suspension, comprises the following steps:
(1) in retort, add concentration to be the dilute sulfuric acid of 0.4M and stir, it is subsequently adding Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 6% and concentration is the sodium dodecyl sulfate aqueous solution of 6%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.07% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.07% of dilute sulfuric acid weight;, it being subsequently adding the Aqueous Solutions of Polyethylene Glycol that fully dispersed concentration is 6%, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.07% of dilute sulfuric acid weight;
(2) in retort with the flow of 1700L/h add modulus be 3.3, concentration be 0.3M water glass solution, it is neutralized reaction while stirring, the strict interpolation speed controlling water glass solution and mixing speed, when the pH value of material system reaches 3.0~4.0, food stage green pigment sorbitol solution is added in retort, its weight is the 0.2% of dilute sulfuric acid, and the pH value controlling reaction end is 4.0~5.0;
(3) continuing to add concentration in retort is the dilute sulfuric acid of 0.4M, the backward retort that stirs is added modulus be 3.3, concentration be the water glass solution of 0.3M, it is neutralized after reaction changes into gel to material system while stirring to stop adding water glass solution, the strict interpolation speed controlling water glass solution and mixing speed, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the green silicon dioxide granule of toothpaste suspension.
Silicon dioxide granule in embodiment 1~6 and comparative example is carried out density and suspension time detection, wherein,
The Chinese patent of comparative example is publication number to be CN100345755, publication date be 2007.10.31 discloses the meansigma methods of embodiment in " preparation method of a kind of nano silicon ".
Suspension time detection process steps is:
First preparing test solution, the component of test solution and mass fraction thereof be: sorbitol 40%, water 55.6%, CMC0.2%, takes 90m test solution in the graduated cylinder of 200ml, and after adding 4g silicon dioxide granule, concussion is uniformly, stands and starts timing.
Testing result is as shown in the table:
As seen from the above table, the density of the silicon dioxide granule prepared by the present invention is significantly lower than prior art, and suspension time is then considerably longer than prior art, and the silicon dioxide granule prepared by the present invention can keep moderate hardness in addition.
Above-described embodiment is illustrative principles of the invention and effect thereof only, not for the restriction present invention.Above-described embodiment all under the spirit and category of the present invention, can be modified or change by any those skilled in the art.Therefore, art has usually intellectual such as modifying without departing from all equivalences completed under disclosed spirit and technological thought or change, must be contained by the claim of the present invention.
Claims (8)
1. the toothpaste preparation method of the colored silicon dioxide granule that suspends, it is characterised in that: comprise the following steps:
(1) in retort, add dilute sulfuric acid and stir, it is subsequently adding fully dispersed Polyethylene Glycol and sodium dodecyl sulfate aqueous solution, the weight of Aqueous Solutions of Polyethylene Glycol is the 0.05~0.1% of dilute sulfuric acid weight, and the weight of sodium dodecyl sulfate aqueous solution is the 0.05~0.1% of dilute sulfuric acid weight;The concentration of described Aqueous Solutions of Polyethylene Glycol is 1~10%, and the concentration of described sodium dodecyl sulfate aqueous solution is 1~10%;
(2) adding water glass solution in retort, be neutralized reaction while stirring, when the pH value of material system reaches 3.0~4.0, add food grade colorant solution in retort, the pH value controlling reaction end is 4.0~5.0;
(3) continue to add dilute sulfuric acid in retort, the backward retort that stirs is added water glass solution, be neutralized after reaction changes into gel to material system while stirring and stop adding water glass solution, obtain silica dioxide gel;
(4) silica dioxide gel that step (3) obtains is carried out filter pressing, obtain gel press cake, with alcoholic solution detergent gel filter cake, and remove the Polyethylene Glycol of sulfate and residual, gel press cake after washing is dried, pulverizes, obtains the colored silicon dioxide granule of toothpaste suspension.
2. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterised in that: in described step (1), the concentration of dilute sulfuric acid is 0.3~0.4M.
3. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterised in that: in described step (2), the modulus of water glass solution is 3.3, and the concentration of water glass solution is 0.3~0.4M.
4. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterised in that: in described step (2), the interpolation speed of water glass solution is 1500~2000L/h.
5. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterized in that: in described step (2), food grade colorant solution is the sorbitol of food stage, glycerol or polyglycol solution, and it adds weight is the 0.1~0.5% of dilute sulfuric acid.
6. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterised in that: in described step (3), the concentration of dilute sulfuric acid is 0.3~0.4M.
7. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterised in that: in described step (3), the modulus of water glass solution is 3.3, and the concentration of water glass solution is 0.3~0.4M.
8. the preparation method of the colored silicon dioxide granule of a kind of toothpaste according to claim 1 suspension, it is characterised in that: in described step (3), the interpolation speed of water glass solution is 1500~2000L/h.
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