CN102530970A - Preparation method of toothpaste abrasive silicon dioxide - Google Patents
Preparation method of toothpaste abrasive silicon dioxide Download PDFInfo
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- CN102530970A CN102530970A CN2012100513253A CN201210051325A CN102530970A CN 102530970 A CN102530970 A CN 102530970A CN 2012100513253 A CN2012100513253 A CN 2012100513253A CN 201210051325 A CN201210051325 A CN 201210051325A CN 102530970 A CN102530970 A CN 102530970A
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Abstract
The invention relates to a preparation method of toothpaste abrasive silicon dioxide. The preparation method comprises the following steps of: in sodium silicate solution with the concentration of 12-15%, adding 10-30% (weight) sulphuric acid according to weight ratio of pure silicon dioxide to concentrated sulfuric acid of being 1: 0.7, reacting for 2-4 hours at the temperature of 40-50 DEG C to generate silicon dioxide gel; adjusting pH value to be 3-5 with sulphuric acid solution with the concentration of 10-30%; adding polyalcohol accounting for 1-3% of the total weight of silicon dioxide, heating to 60-80 DEG C, insulating for 1-3 hours and carrying out structural control; then filtering, washing, carrying out high pressure beating on filter cakes, curing, and then drying and smashing until average particle size is 8-10Mum. In the invention, the polyalcohol is taken as a structural control agent, the prepared silicon dioxide has appropriate hardness and moderate abrasiveness when being used as toothpaste abrasive, does no harm to gum and has good toothpaste transparency; meanwhile raw materials are available, cost is low, process flow is short, and industrialization is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation method of toothpaste abrasives silicon-dioxide.
Background technology
Abrasive is content is maximum in the toothpaste composition, mainly plays the effect of cleaning teeth, and most at present toothpaste all are to process with the abrasive of single component, like lime carbonate, silicon-dioxide, white lake, secondary calcium phosphate, Calcium Pyrophosphate etc.China is widely used light calcium carbonate as toothpaste abrasive, but these abrasives are to there being some injuries to gum, the raising of Along with people's living standard and health perception, and the transparent toothpaste with silicon-dioxide of suitable abrasivity receives popular welcome.Wet production silicon-dioxide is divided into the gel method and the precipitator method at present; Because gel method silicon-dioxide kind is single; Mainly be to use at present the silicon-dioxide of precipitator method preparation to use as friction agent, the precipitator method are produced silicon-dioxide normally with the vitriol oil and water glass, add in the reaction kettle respectively according to weight proportion and react; Again through filtration, washing, filter cake through high pressure making beating, slaking, be stored in the underflow jar, then through dry silicon-dioxide.For example to disclose the friction agent that a kind of " gel dentifrice of visually clear " wherein add be a kind of precipitated silica to patent CN1079383A; But the toothpaste that this precipitated silica is processed as friction agent still has higher abrasivity, and transparency also receives certain influence.
Summary of the invention
The objective of the invention is to the existing precipitator method are produced the improvement of the shortcoming of friction agent existence, the preparation method of another kind of toothpaste abrasives silicon-dioxide is provided.Toothpaste transparency to realize preparation is higher, and abrasivity is suitable; And raw material is easy to get, and is cheap, and flow process is short, is easy to realize industriallization.
Preparing method of the present invention may further comprise the steps:
(1) deposition: in concentration is in the sodium silicate solution of 12-15%, according to pure silicon dioxide: the weight ratio=1:0.7 of the vitriol oil, add 10～30% sulfuric acid (weight), under temperature 40-50 ℃, react 2-4 hour the generation silica dioxide gel;
(2) structure control: using concentration is the sulphuric acid soln of 10～30% (weight), adjustment pH value 3-5; Add the polyvalent alcohol of silicon-dioxide gross weight 1-3%, be warming up to 60-80 ℃, be incubated 1-3 hour;
(3) it is below 0.2% that filtration, deposition water are washed till sodium ions content; Filter cake was pulled an oar 1-2 hour under 2300-2700 rev/min with high speed dispersor;
(4) drying: at 100-400 ℃ of quick dewatering drying; Being crushed to mean particle size again is the 8-10 micron.
Said polyvalent alcohol is one or more of terepthaloyl moietie, glycerine, sorbyl alcohol, tetramethylolmethane.
The rotating speed of said high speed dispersor is 2300-2700 rev/min.
Said quick dewatering drying is an expansion drying.
It is constitution controller that the present invention adopts polyvalent alcohol, and its dioxide-containing silica of silicon-dioxide of this method preparation is more than 99.6%, mean particle size: 8-10 μ m; Be used for toothpaste abrasives and have suitable hardness, its dentin abrasion value (RADRDA) reaches 70-120, and the product pore volume of processing is 0.9-1.5ml/g, and the BET specific surface area is 500-600m
2/ g, the toothpaste transparency is good, and abrasivity is moderate, can not damage gum.And this silicon-dioxide has variety, can be used in the toothpaste of different performance.And raw material is prone to, and is cheap, and flow process is short, is easy to realize industriallization.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1:
The weight percent of preparation silicon-dioxide is 12% sodium silicate solution 500g, under 40 ℃ of temperature
Add the sulphuric acid soln 210g of 20% (weight), reacted 2 hours, adjusting pH value with the sulfuric acid of 20% (weight) is 3-4; Add terepthaloyl moietie 0.6g, be warming up to 70 ℃ of insulations 2 hours;
Filter cake after washing, will washing utilizes high speed dispersor under 2700 rev/mins again, filter cake is pulled an oar disperseed 1 hour; Expansion drying also is crushed to granularity 8-10 micron and obtains toothpaste abrasives silicon-dioxide;
Its physical and chemical performance is following
Embodiment 1: toothpaste abrasives silicon-dioxide physical and chemical performance table
Embodiment 2;
The preparation dioxide-containing silica is the sodium silicate solution 500g of 15% (weight), at 50 ℃ of sulfuric acid (weight) solution 515g that add preparation 10% down of temperature, reacts 4 hours; Use sulfuric acid adjustment pH value for being 3-4; Add sorbyl alcohol 1.5g, be warming up to 80 ℃, be incubated one hour; Through filtering, wash and utilizing high speed dispersor under 2600 rev/mins, filter cake is pulled an oar disperseed 1 hour again; Adopt expansion drying and pulverize the toothpaste abrasives silicon-dioxide that obtains mean particle size 9-10 micron.Its experimental data is following.
Embodiment 2: toothpaste abrasives silicon-dioxide physical and chemical performance table
Embodiment 3:
The preparation dioxide-containing silica is 13
The sodium silicate solution 500g of % (weight) at 50 ℃ of sulfuric acid (weight) solution 303g that add preparation 15% down of temperature, reacted 3 hours, used sulfuric acid adjustment pH value for being 4-5, added tetramethylolmethane 1.5g, was warming up to 80 ℃, was incubated one hour; Through filtering, wash and utilizing high speed dispersor under 2400 rev/mins, filter cake is pulled an oar disperseed 1.5 hours again; Adopt
Expansion drying and pulverizing obtain the toothpaste abrasives silicon-dioxide of mean particle size 8-10 micron.Its experimental data is following.
Embodiment 3: toothpaste abrasives silicon-dioxide physical and chemical performance table
Embodiment 4
The preparation dioxide-containing silica is the sodium silicate solution 500g of 14% (weight), at 40 ℃ of sulfuric acid (weight) solution 163g that add preparation 30% down of temperature, reacts 2 hours; Use sulfuric acid adjustment pH value for being 4-5; Add glycerine 1.0g, be warming up to 80 ℃, be incubated one hour; Through filtering, wash and utilizing high speed dispersor under 2300 rev/mins, filter cake is pulled an oar disperseed 2 hours again; Adopt
Expansion drying and pulverizing obtain the toothpaste abrasives silicon-dioxide of mean particle size 8-9 micron.Its experimental data is following.
Embodiment 4: cream friction agent silicon-dioxide physical and chemical performance table
Embodiment 5
The preparation dioxide-containing silica is the sodium silicate solution 500g of 14% (weight), at 40 ℃ of sulfuric acid (weight) solution 163g that add preparation 30% down of temperature, reacts 2 hours; Use sulfuric acid adjustment pH value for being 4-5; Add terepthaloyl moietie, each 0.5 g of glycerine, be warming up to 80 ℃, be incubated one hour; Through filtering, wash and utilizing high speed dispersor under 2300 rev/mins, filter cake is pulled an oar disperseed 2 hours again; Adopt
Expansion drying and pulverizing obtain the toothpaste abrasives silicon-dioxide of mean particle size 8-9 micron.Its experimental data is following.
Embodiment 5: cream friction agent silicon-dioxide physical and chemical performance table
Claims (4)
1. the preparation method of a toothpaste abrasives silicon-dioxide is characterized in that, may further comprise the steps:
(1) deposition: in concentration is in the sodium silicate solution of 12-15%, and according to pure silicon dioxide: vitriol oil weight ratio=1:0.7 adds the sulfuric acid of 10～30% (weight), under temperature 40-50 ℃, react 2-4 hour the generation silica dioxide gel;
(2) structure control: using concentration is the sulphuric acid soln of 10～30% (weight), adjustment pH value 3-5; Add the polyvalent alcohol of silicon-dioxide gross weight 1-3%, be warming up to 60-80 ℃, be incubated 1-3 hour;
(3) it is below 0.2% that filtration, deposition water are washed till sodium ions content; With high speed dispersor filter cake was pulled an oar 1-2 hour;
(4) drying: at 100-400 ℃ of quick dewatering drying; Being crushed to mean particle size again is the 8-10 micron.
2. the preparation method of toothpaste abrasives silicon-dioxide according to claim 1 is characterized in that, said polyvalent alcohol is one or more of terepthaloyl moietie, glycerine, sorbyl alcohol, tetramethylolmethane.
3. the preparation method of toothpaste abrasives silicon-dioxide according to claim 1 is characterized in that, the rotating speed of said high speed dispersor is 2300-2700 rev/min.
4. the preparation method of toothpaste abrasives silicon-dioxide according to claim 1 is characterized in that, said quick dewatering drying is an expansion drying.
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| CN201210051325.3A CN102530970B (en) | 2012-03-01 | 2012-03-01 | Preparation method of toothpaste abrasive silicon dioxide |
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| CN201210051325.3A CN102530970B (en) | 2012-03-01 | 2012-03-01 | Preparation method of toothpaste abrasive silicon dioxide |
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| CN102530970B CN102530970B (en) | 2014-02-19 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103690382A (en) * | 2013-12-26 | 2014-04-02 | 福建龙岩精博化工科技有限公司 | Preparation technology of environment-friendly toothpaste abrasive |
| CN103730633A (en) * | 2013-12-13 | 2014-04-16 | 垦利三合新材料科技有限责任公司 | Preparation method for anode material of high-capacity power lithium-ion secondary battery |
| CN104528738A (en) * | 2014-12-23 | 2015-04-22 | 肇庆金三江硅材料有限公司 | Method for preparing low-wear silica particles for toothpaste |
| CN104528739A (en) * | 2014-12-23 | 2015-04-22 | 广州市飞雪材料科技有限公司 | Preparation method of high-refractive-index high-transparency friction type silicon dioxide |
| CN104944429A (en) * | 2015-06-26 | 2015-09-30 | 肇庆学院 | Compound silicon dioxide and preparation method thereof and appliance in toothpaste |
| CN107792861A (en) * | 2017-11-06 | 2018-03-13 | 广州市飞雪材料科技有限公司 | A kind of low index of refraction high transparency friction type silica and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103730633A (en) * | 2013-12-13 | 2014-04-16 | 垦利三合新材料科技有限责任公司 | Preparation method for anode material of high-capacity power lithium-ion secondary battery |
| CN103730633B (en) * | 2013-12-13 | 2017-07-18 | 垦利三合新材料科技有限责任公司 | A kind of preparation method of high-capacity dynamical lithium-ion secondary battery cathode material |
| CN103690382A (en) * | 2013-12-26 | 2014-04-02 | 福建龙岩精博化工科技有限公司 | Preparation technology of environment-friendly toothpaste abrasive |
| CN104528738A (en) * | 2014-12-23 | 2015-04-22 | 肇庆金三江硅材料有限公司 | Method for preparing low-wear silica particles for toothpaste |
| CN104528739A (en) * | 2014-12-23 | 2015-04-22 | 广州市飞雪材料科技有限公司 | Preparation method of high-refractive-index high-transparency friction type silicon dioxide |
| CN104528739B (en) * | 2014-12-23 | 2016-03-16 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high refractive index high transparency friction type silicon-dioxide |
| CN104944429A (en) * | 2015-06-26 | 2015-09-30 | 肇庆学院 | Compound silicon dioxide and preparation method thereof and appliance in toothpaste |
| CN104944429B (en) * | 2015-06-26 | 2017-03-01 | 肇庆学院 | A kind of compound silicon dioxide and preparation method thereof and its application in toothpaste |
| CN107792861A (en) * | 2017-11-06 | 2018-03-13 | 广州市飞雪材料科技有限公司 | A kind of low index of refraction high transparency friction type silica and its preparation method and application |
| US10406084B2 (en) | 2017-11-06 | 2019-09-10 | Guangzhou Feixue Material Technology Co., Ltd. | Low refractive index, high transparency, and abrasive type silica, preparation method and application thereof |
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