CN104528739A - Preparation method of high-refractive-index high-transparency friction type silicon dioxide - Google Patents
Preparation method of high-refractive-index high-transparency friction type silicon dioxide Download PDFInfo
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Abstract
The invention provides a preparation method of high-refractive-index high-transparency friction type silicon dioxide. The preparation method comprises the following steps: (1) blending a sodium silicate solution, adding a surfactant, and stirring uniformly; (2) injecting sodium sulfate solution into a reaction tank, starting a stirring device, and heating to 80-90 DEG C; (3) adding the sodium silicate solution into the reaction tank, synchronously adding sulfuric acid solution after 0.5-1 minute, controlling a pH value to be 9.0-9.5, further adding the sulfuric acid solution after the sodium silicate solution is completely added, controlling the pH value of a reaction end point to be 4.4-4.8, then stopping adding the sulfuric acid solution, keeping temperature at 80-85 DEG C, and further stirring and precipitating for 10-15 minutes to obtain slurry; and (4) performing pressure filtration on the slurry obtained in the step (3) to obtain a filter cake, washing the filter cake by using deionized water, and drying and crushing the washed filter cake to obtain high-refractive-index high-transparency friction type silicon dioxide. Silicon dioxide prepared by using the method provided by the invention is high in refractive index and wide in range, ensures that the transparency can reach 99.0%, and also has good cleaning performance and fluorine compatibility.
Description
Technical field
The invention belongs to toothpaste production silicon-dioxide, be specifically related to a kind of preparation method of high refractive index high transparency friction type silicon-dioxide.
Background technology
Features such as silicon-dioxide is stablized because having physicochemical property, cleaning capacity is strong, the preparation that can be used for transparent toothpaste good with toothpaste Miscibility and being widely used in toothpaste industry.Silicon-dioxide in toothpaste as abrasive material and thickening material.
The transmittance of silicon-dioxide is higher, and the transparency of lotion of toothpaste is better.The refreshing heart is pleasing, the sensation of clean and safe because the outward appearance of its uniqueness is brought to human consumer for transparent toothpaste, be well received by consumers, but not every silicon-dioxide can be used for the preparation of transparent toothpaste, must ensure that the refractive index of this silicon-dioxide is consistent with toothpaste liquid phase refractive index, this just requires that silicon-dioxide has the refractive index of more Gao Gengkuan.Toothpaste friction type silicon-dioxide transparency under the refractive index of 1.435-1.46 that traditional technology is produced is up to 94%, in this is interval transparency 1.447 refractive index be issued to the highest after start decline, and downtrending is obvious, add formulation of tooth-paste research difficulty, and be not suitable for the formulation of tooth-paste high to transparency requirement.The many emphasis of production technique of current toothpaste friction type silicon-dioxide make clear of the raising of lightness, but still do not have effective solution for transparency change parabolically under certain refractive index scope.Silicon-dioxide can reduce along with increasing transparency of its friction valve, how to ensure that the situation not affecting frictional behaviour is issued to high-clarity, is toothpaste industry problem demanding prompt solution.
Chinese patent CN104030303A discloses a kind of production method of Silica Using for Toothpaste abrasive, and its step comprises: in reaction vessel, add deionized water, sodium salt and anion surfactant, stir; Pressure in adjustment reaction vessel is 0.15-0.5Mpa, and temperature is 110-150 DEG C, then in reaction vessel, adds water glass and dilute acid soln simultaneously, and the speed that adds of adjustment water glass and dilute acid soln makes the solution ph in reaction vessel control at 9.0-9.2; After having reacted, in reactor, add dilute acid soln, being acidified to pH value in reaction is 3.5 ± 0.2; After acidifying completes, by the solution left standstill ageing in reactor, then successively by press filtration, washing, slurrying, spraying dry, pulverizing, obtain Silica Using for Toothpaste abrasive.The anion surfactant that this invention uses is Sodium Lauryl Sulphate BP/USP and/or sodium lauryl sulphate.The object of this invention is to improve product coefficient of friction and granule strength, and with no specific disclosure of its refractive index, transparency, therefore the unpromising the present invention of this invention brings technology to enlighten.
In sum, in order to solve a difficult problem for prior art, develop that a kind of refractive index is high, transparency is high and the friction type silicon-dioxide with good clean-up performance seems and is even more important.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of high refractive index high transparency friction type silicon-dioxide, the refractive index of the silicon-dioxide prepared is high, within the scope of 1.435-1.458 refractive index, transparency is up to 99%, and it is not obvious to reach the highest rear fall in this interval transparency, also has good clean-up performance and fluorine consistency simultaneously.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for high refractive index high transparency friction type silicon-dioxide, comprises the following steps:
(1) allocate sodium silicate solution, add tensio-active agent, stir;
(2) inject metabisulfite solution toward retort, open whipping appts, be heated to 80-90 DEG C;
(3) in retort, sodium silicate solution is added, add sulphuric acid soln after 0.5-1min simultaneously, control pH value at 9.0-9.5, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.4-4.8, stop adding sulphuric acid soln, keep temperature 80-85 DEG C, continue to stir precipitation 10-15min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely obtain high refractive index high transparency friction type silicon-dioxide.
Further, the volume ratio of described metabisulfite solution and described sodium silicate solution is 1:(1.0-1.3).
Further, the concentration of the sodium silicate solution in described step (1) is 2.0-2.5M.
Further, the addition of the tensio-active agent in described step (1) is described sodium silicate solution volume (m
3) 1.0-2.0%(kg).
Further, the tensio-active agent in described step (1) is the combination of one or more in sodium lauryl sulphate, N-lauroyl ALANINE sodium, citrate salt APA, polyoxyethylene glycol (600) bilaurate, cocamidopropyl propyl amide amine oxide and ethoxylated dodecyl alcohol sodium sulfate.As the preferred embodiment of the present invention, described tensio-active agent is the mixture of cocamidopropyl propyl amide amine oxide and sodium lauryl sulphate, and the Mixing ratio by weight of described cocamidopropyl propyl amide amine oxide and sodium lauryl sulphate is 1:1.5.
Further, in described step (2), the concentration of metabisulfite solution is 2.5-4.5%.
Further, the interpolation flow of described step (3) mesosilicic acid sodium solution is 12-16m3/h.
Above-mentioned sodium lauryl sulphate is white or faint yellow powdery, and molecular-weight average is 288, is a kind of anion surfactant, its biological degradability >90%.Because of its have foaming, emulsification, infiltration effect and be used to toothpaste preparation.
Above-mentioned N-lauroyl ALANINE sodium, be the anion surfactant of a kind of non-toxic and safe, readily biodegradable, its surfactivity and penetrating quality are better than sodium lauryl sulphate.
Above-mentioned citrate salt APA is colourless transparent liquid, and active matter content is 30%, is a kind of anion surfactant of performance gentleness.
Above-mentioned polyoxyethylene glycol (600) bilaurate is white or faint yellow solid, and water-soluble, compatibleness is good, and molecular weight is 540-660, and zero pour is 20-25 DEG C, hydroxyl value 170-208(mgKOH/g), be a kind of nonionogenic tenside.Can be used for the preparation of transparent toothpaste.
Above-mentioned cocamidopropyl propyl amide amine oxide is colourless transparent liquid, and active matter content soluble in water is 30.0 ± 2.0%, efficient whipping agent and stablizer, is a kind of cats product.
Above-mentioned ethoxylated dodecyl alcohol sodium sulfate is oyster white paste, and relative molecular weight is 462, and HLB value is 16.5, and cloud point (10% aqueous solution) is 100 DEG C, is a kind of anion surfactant.
Compared with prior art, the present invention has following beneficial effect:
High refractive index high transparency friction type silicon-dioxide silicon-dioxide of the present invention take metabisulfite solution as reaction promoter, take water glass as silicon source, neutralization reaction is carried out with sulfuric acid, tensio-active agent is utilized to carry out modification as properties-correcting agent, and be precipitated silicon-dioxide by the pH value in control reaction process and temperature of reaction, under the silicon-dioxide high refractive index of the rear gained of dry screening, transparency improves, transparency within the scope of 1.435-1.46 refractive index can up to 99.0%, wherein between 1.435-1.450 refractive index, transparency progressively rises, under 1.450 refractive index, transparency can reach 99.0%, 1.450-1.458 under every bit refractive index, transparency change trend is little in interval.Adding of tensio-active agent of the present invention can form adsorption layer in solid-liquid interface, reduce interfacial free energy, change surface properties and the microtexture of solid particulate, make it easy dispersion, be conducive to the formation of electrostatic double layer around particle simultaneously, hinder particle accumulation by Coulomb repulsion, uniform particles is little with the raising and variation tendency thereof that ensure transparency, and the tensio-active agent non-toxic and safe that the present invention adopts, react rear unnecessary tensio-active agent and be easily removed, harmless to human-body safety.Meanwhile, the silicon-dioxide oil-absorption(number) that the present invention prepares is 90-120ml/100g, meets the industry requirement of friction type Silica Using for Toothpaste; Apparent density > 0.3g/ml, fluorine consistency > 90%, have good compatibleness, at the good dispersity of toothpaste system, is applicable to all types of toothpaste, especially can be used for the preparation of super transparent toothpaste.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
embodiment 1
A preparation method for high refractive index high transparency friction type silicon-dioxide, comprises the following steps:
(1) allocating concentration is 2.0M sodium silicate solution 10m
3, add 1.0kg tensio-active agent, stir, described tensio-active agent is the mixture that sodium lauryl sulphate and ethoxylated dodecyl alcohol sodium sulfate are mixed to get with weight ratio 1:1;
(2) past retort implantation concentration is 2.5% metabisulfite solution 10m
3, open whipping appts, be heated to 80 DEG C;
(3) in retort, sodium silicate solution is added with the flow of 12m3/h, add sulphuric acid soln after 0.5min simultaneously, control pH value 9.0, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.4, stop adding sulphuric acid soln, keep temperature 80 DEG C, continue to stir precipitation 10min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely arrive high refractive index high transparency friction type silicon-dioxide.
embodiment 2
A preparation method for high refractive index high transparency friction type silicon-dioxide, comprises the following steps:
(1) allocating concentration is 2.5M sodium silicate solution 13m
3, add 2.0kg tensio-active agent, stir, described tensio-active agent is the mixture that sodium lauryl sulphate and polyoxyethylene glycol (600) bilaurate are mixed to get with weight ratio 1:1;
(2) past retort implantation concentration is 4.5% metabisulfite solution 10m
3, open whipping appts, be heated to 90 DEG C;
(3) in retort, sodium silicate solution is added with the flow of 16m3/h, add sulphuric acid soln after 1min simultaneously, control pH value 9.5, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.8, stop adding sulphuric acid soln, keep temperature 85 DEG C, continue to stir precipitation 15min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely arrive high refractive index high transparency friction type silicon-dioxide.
embodiment 3
A preparation method for high refractive index high transparency friction type silicon-dioxide, comprises the following steps:
(1) allocating concentration is 2.3M sodium silicate solution 11m
3, add 1.5kg tensio-active agent, stir, described tensio-active agent is the mixture that cocamidopropyl propyl amide amine oxide and sodium lauryl sulphate are mixed to get with weight ratio 1:1.5;
(2) past retort implantation concentration is 3.5% metabisulfite solution 10m
3, open whipping appts, be heated to 85 DEG C;
(3) in retort, sodium silicate solution is added with the flow of 14m3/h, add sulphuric acid soln after 0.5min simultaneously, control pH value 9.3, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.5, stop adding sulphuric acid soln, keep temperature 85 DEG C, continue to stir precipitation 10min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely arrive high refractive index high transparency friction type silicon-dioxide.
embodiment 4
A preparation method for high refractive index high transparency friction type silicon-dioxide, comprises the following steps:
(1) allocating concentration is 2.3M sodium silicate solution 11m
3, add 1.5kg tensio-active agent, stir, described tensio-active agent is sodium lauryl sulphate;
(2) past retort implantation concentration is 3.5% metabisulfite solution 10m
3, open whipping appts, be heated to 85 DEG C;
(3) in retort, sodium silicate solution is added with the flow of 14m3/h, add sulphuric acid soln after 0.5min simultaneously, control pH value 9.3, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.5, stop adding sulphuric acid soln, keep temperature 85 DEG C, continue to stir precipitation 10min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely arrive high refractive index high transparency friction type silicon-dioxide.
embodiment 5
A preparation method for high refractive index high transparency friction type silicon-dioxide, comprises the following steps:
(1) allocating concentration is 2.3M sodium silicate solution 11m
3, add 1.5kg tensio-active agent, stir, described tensio-active agent is cocamidopropyl propyl amide amine oxide;
(2) past retort implantation concentration is 3.5% metabisulfite solution 10m
3, open whipping appts, be heated to 85 DEG C;
(3) in retort, sodium silicate solution is added with the flow of 14m3/h, add sulphuric acid soln after 0.5min simultaneously, control pH value 9.3, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.5, stop adding sulphuric acid soln, keep temperature 85 DEG C, continue to stir precipitation 10min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely arrive high refractive index high transparency friction type silicon-dioxide.
experimental example one
The silicon-dioxide obtained to embodiment 1 ~ 5 detects, and detected result is as shown in the table:
As seen from the above table, the transparency in the interval of refractive index 1.444-1.450 of the silicon-dioxide prepared by the present invention improves gradually, and the highest in refractive index 1.450 times transparencies, in 1.450-1.458 interval, under every bit refractive index, transparency change trend is little.Wherein embodiment 1-3 all reaches more than 98%, especially the highest with the transparency of embodiment 3, is 99.0%, and the transparency of embodiment 4 and 5 silicon-dioxide is high not as good as embodiment 3, illustrates that cocamidopropyl propyl amide amine oxide and sodium lauryl sulphate have good synergy.Preparation method of the present invention can keep higher fluorine consistency simultaneously, can reach more than 90%; Oil-absorption(number), between 90-120ml/100g, meets the industry requirement of friction type Silica Using for Toothpaste, has good clean-up performance; At the good dispersity of toothpaste system, stable performance, is applicable to all types of toothpaste, especially can be used for the preparation of super transparent toothpaste.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (8)
1. a preparation method for high refractive index high transparency friction type silicon-dioxide, is characterized in that, comprise the following steps:
(1) allocate sodium silicate solution, add tensio-active agent, stir;
(2) inject metabisulfite solution toward retort, open whipping appts, be heated to 80-90 DEG C;
(3) in retort, sodium silicate solution is added, add sulphuric acid soln after 0.5-1min simultaneously, control pH value at 9.0-9.5, the pH value continuing to add sulphuric acid soln control reaction end after sodium silicate solution adds is 4.4-4.8, stop adding sulphuric acid soln, keep temperature 80-85 DEG C, continue to stir precipitation 10-15min, obtain slurry;
(4) slurry that step (3) obtains is carried out press filtration, obtain filter cake, use deionized water wash filter cake, to the filtration cakes torrefaction after washing, pulverizing, namely obtain high refractive index high transparency friction type silicon-dioxide.
2. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 1, it is characterized in that, the volume ratio of described metabisulfite solution and described sodium silicate solution is 1:(1.0-1.3).
3. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 1, it is characterized in that, the concentration of the sodium silicate solution in described step (1) is 2.0-2.5M.
4. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 1, it is characterized in that, the addition of the tensio-active agent in described step (1) is the 1.0-2.0% of described sodium silicate solution volume.
5. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 1, it is characterized in that, the tensio-active agent in described step (1) is the combination of one or more in sodium lauryl sulphate, N-lauroyl ALANINE sodium, citrate salt APA, polyoxyethylene glycol (600) bilaurate, cocamidopropyl propyl amide amine oxide and ethoxylated dodecyl alcohol sodium sulfate.
6. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 5, it is characterized in that, described tensio-active agent is the mixture of cocamidopropyl propyl amide amine oxide and sodium lauryl sulphate, and the Mixing ratio by weight of described cocamidopropyl propyl amide amine oxide and sodium lauryl sulphate is 1:1.5.
7. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 1, is characterized in that, in described step (2), the concentration of metabisulfite solution is 2.5-4.5%.
8. the preparation method of high refractive index high transparency friction type silicon-dioxide as claimed in claim 1, it is characterized in that, the interpolation flow of described step (3) mesosilicic acid sodium solution is 12-16m3/h.
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| CN106276929A (en) * | 2016-07-29 | 2017-01-04 | 广州市飞雪材料科技有限公司 | A kind of preparation method of the type silicon dioxide that rubs |
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| CN104528739B (en) | 2016-03-16 |
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