CN102530970B - Preparation method of toothpaste abrasive silicon dioxide - Google Patents
Preparation method of toothpaste abrasive silicon dioxide Download PDFInfo
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- CN102530970B CN102530970B CN201210051325.3A CN201210051325A CN102530970B CN 102530970 B CN102530970 B CN 102530970B CN 201210051325 A CN201210051325 A CN 201210051325A CN 102530970 B CN102530970 B CN 102530970B
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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 silica for toothpaste abrasive agent.
Background technology
Abrasive is composition that in toothpaste, content is maximum, the effect of mainly playing cleaning teeth, and most toothpaste is all to make with the abrasive of single component at present, as calcium carbonate, silicon-dioxide, aluminium hydroxide, secondary calcium phosphate, Calcium Pyrophosphate etc.China is widely used light calcium carbonate as toothpaste abrasive, but these abrasives to gum is had some injury, along with the raising of people's living standard and health perception, the transparent toothpaste with the silicon-dioxide of suitable abrasivity is welcomed by the general public.Wet production silicon-dioxide is divided into gel method and the precipitator method at present, because gel method silicon-dioxide kind is single, at present be mainly that the silicon-dioxide that uses the precipitator method to prepare is used as friction agent, the precipitator method are produced silicon-dioxide normally by the vitriol oil and water glass, according to weight proportion, add in reactor and react respectively, again after filtration, washing, filter cake through high pressure making beating, slaking, be stored in underflow tank, then drying obtains 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 made as friction agent still has higher removal erosion degree, and transparency is also subject to certain impact.
Summary of the invention
The object of the invention is to the existing precipitator method to produce the improvement of the shortcoming of friction agent existence, the preparation method of another kind of silica for toothpaste abrasive agent is provided.Higher to realize the toothpaste transparency of preparing, abrasivity is suitable; And raw material is easy to get, cheap, flow process is short, is easy to realize industrialization.
Preparation method of the present invention comprises the following steps:
(1) precipitation: in the sodium silicate solution that is 12-15% in concentration, according to pure silicon dioxide: the weight ratio=1:0.7 of the vitriol oil, add 10～30% sulfuric acid (weight), at temperature 40-50 ℃, reaction 2-4 hour, generates silica dioxide gel;
(2) structure control: be the sulphuric acid soln of 10～30% (weight) by concentration, adjust pH value 3-5; The polyvalent alcohol that adds silicon-dioxide gross weight 1-3%, is warming up to 60-80 ℃, insulation 1-3 hour;
(3) filter, precipitation wash with water to sodium ions content be below 0.2%; 1-2 hour pulls an oar filter cake under 2300-2700 rev/min with high speed dispersor;
(4) dry: at 100-400 ℃ of quick dewatering drying; Being crushed to mean particle size is 8-10 micron again.
Described polyvalent alcohol is one or more of ethylene glycol, glycerine, sorbyl alcohol, tetramethylolmethane.
The rotating speed of described high speed dispersor is 2300-2700 rev/min.
Described quick dewatering drying is expansion drying.
It is constitution controller that the present invention adopts polyvalent alcohol, and its dioxide-containing silica of silicon-dioxide prepared by this method is more than 99.6%, mean particle size: 8-10 μ m; For toothpaste abrasives, have suitable hardness, its dentin abrasion value (RADRDA) reaches 70-120, and the product pore volume of making is 0.9-1.5ml/g, and BET specific surface area is 500-600m
2/ g, toothpaste transparency is good, and abrasivity is moderate, can not damage gum.And this silicon-dioxide has diversity, can be used in the toothpaste of different performance.And raw material is easy, cheap, flow process is short, is easy to realize industrialization.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
The sodium silicate solution 500g that the weight percent of preparation silicon-dioxide is 12%, at 40 ℃ of temperature
Add 20%(weight) sulphuric acid soln 210g, react, use 20%(weight 2 hours) sulfuric acid to adjust pH value be 3-4; Add ethylene glycol 0.6g, be warming up to 70 ℃ of insulations 2 hours;
Through washing, utilizing high speed dispersor under 2700 revs/min the filter cake after washing, filter cake is pulled an oar and disperseed 1 hour again; Expansion drying is also crushed to granularity 8-10 micron and obtains silica for toothpaste abrasive agent;
Its physical and chemical performance is as follows
Embodiment 1: silica for toothpaste abrasive agent physical and chemical performance table
Embodiment 2;
Preparation dioxide-containing silica is 15%(weight) sodium silicate solution 500g, under temperature 50 C, add preparation 10% sulfuric acid (weight) solution 515g, react 4 hours, with sulfuric acid, adjust pH value for being 3-4, add sorbyl alcohol 1.5g, be warming up to 80 ℃, be incubated one hour; Again after filtration, wash and utilize high speed dispersor under 2600 revs/min, filter cake is pulled an oar and is disperseed 1 hour; Adopt expansion drying and pulverize the silica for toothpaste abrasive agent that obtains mean particle size 9-10 micron.Its experimental data is as follows.
Embodiment 2: silica for toothpaste abrasive agent physical and chemical performance table
Embodiment 3:
Preparation dioxide-containing silica is 13
%(weight) sodium silicate solution 500g adds sulfuric acid (weight) the solution 303g for preparing 15% under temperature 50 C, reacts 3 hours, with sulfuric acid, adjusts pH value for being 4-5, adds tetramethylolmethane 1.5g, is warming up to 80 ℃, is incubated one hour; Again after filtration, wash and utilize high speed dispersor under 2400 revs/min, filter cake is pulled an oar and is disperseed 1.5 hours; Adopt
Expansion drying and pulverizing obtain the silica for toothpaste abrasive agent of mean particle size 8-10 micron.Its experimental data is as follows.
Embodiment 3: silica for toothpaste abrasive agent physical and chemical performance table
Embodiment 4
Preparation dioxide-containing silica is 14%(weight) sodium silicate solution 500g, at 40 ℃ of temperature, add sulfuric acid (weight) the solution 163g of preparation 30%, react 2 hours, with sulfuric acid, adjust pH value for being 4-5, add glycerine 1.0g, be warming up to 80 ℃, be incubated one hour; Again after filtration, wash and utilize high speed dispersor under 2300 revs/min, filter cake is pulled an oar and is disperseed 2 hours; Adopt
Expansion drying and pulverizing obtain the silica for toothpaste abrasive agent of mean particle size 8-9 micron.Its experimental data is as follows.
Embodiment 4: cream friction agent silicon-dioxide physical and chemical performance table
Embodiment 5
Preparation dioxide-containing silica is 14%(weight) sodium silicate solution 500g, at 40 ℃ of temperature, add sulfuric acid (weight) the solution 163g of preparation 30%, react 2 hours, with sulfuric acid, adjust pH value for being 4-5, add ethylene glycol, each 0.5 g of glycerine, be warming up to 80 ℃, be incubated one hour; Again after filtration, wash and utilize high speed dispersor under 2300 revs/min, filter cake is pulled an oar and is disperseed 2 hours; Adopt
Expansion drying and pulverizing obtain the silica for toothpaste abrasive agent of mean particle size 8-9 micron.Its experimental data is as follows.
Embodiment 5: cream friction agent silicon-dioxide physical and chemical performance table
Claims (4)
1. a preparation method for silica for toothpaste abrasive agent, is characterized in that, comprises the following steps:
(1) precipitation: in the sodium silicate solution that the mass percent of silicon-dioxide is 12-15%, according to pure silicon dioxide: vitriol oil weight ratio=1:0.7 adds the sulfuric acid of 10～30% weight, and at temperature 40-50 ℃, reaction 2-4 hour, generates silica dioxide gel;
(2) structure control: be the sulphuric acid soln of 10～30% weight by concentration, adjust pH value 3-5; The polyvalent alcohol that adds silicon-dioxide gross weight 1-3%, is warming up to 60-80 ℃, insulation 1-3 hour;
(3) filter, precipitation wash with water to sodium ions content be below 0.2%; With high speed dispersor by the filter cake 1-2 hour that pulls an oar;
(4) dry: at 100-400 ℃ of quick dewatering drying; Being crushed to mean particle size is 8-10 micron again.
2. the preparation method of silica for toothpaste abrasive agent according to claim 1, is characterized in that, described polyvalent alcohol is one or more of ethylene glycol, glycerine, sorbyl alcohol, tetramethylolmethane.
3. the preparation method of silica for toothpaste abrasive agent according to claim 1, is characterized in that, the rotating speed of described high speed dispersor is 2300-2700 rev/min.
4. the preparation method of silica for toothpaste abrasive agent according to claim 1, is characterized in that, described quick dewatering drying is 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 true CN102530970B (en) | 2014-02-19 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN104528738B (en) * | 2014-12-23 | 2016-01-20 | 连云港金三江硅材料有限公司 | A kind of preparation method of low wearing and tearing Silica Using for Toothpaste particle |
| 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 |
| CN107792861B (en) * | 2017-11-06 | 2018-08-28 | 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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|---|---|---|---|---|
| CN1221393A (en) * | 1996-06-06 | 1999-06-30 | 罗狄亚化学公司 | Silica capable of being used in toothpaste composition |
| CN102002120A (en) * | 2010-09-20 | 2011-04-06 | 中国海洋石油总公司 | Method for preparing special silica gel carrier with large pore volume and large specific surface area |
| CN102145897A (en) * | 2011-04-19 | 2011-08-10 | 冷水江三A化工有限责任公司 | Large-pore-volume silicon dioxide with nanoparticle structure and preparation method thereof |
| CN102167337A (en) * | 2011-03-21 | 2011-08-31 | 冷水江三A化工有限责任公司 | Silicon dioxide aerogel and preparation method thereof |
| CN102199378A (en) * | 2011-03-21 | 2011-09-28 | 冷水江三A化工有限责任公司 | Preparation method for silica aerogel flatting agent |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6977065B1 (en) * | 1993-10-07 | 2005-12-20 | Degussa Ag | Precipitated silicas |
| FR2809955B1 (en) * | 2000-06-07 | 2004-11-26 | Rhodia Chimie Sa | USE OF A HIGH STRUCTURE, DENSE AND DISPERSIBLE PRECIPITATION SILICA AS A THICKENING OR TEXTURING AGENT IN TOOTHPASTE COMPOSITIONS |
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- 2012-03-01 CN CN201210051325.3A patent/CN102530970B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221393A (en) * | 1996-06-06 | 1999-06-30 | 罗狄亚化学公司 | Silica capable of being used in toothpaste composition |
| CN102002120A (en) * | 2010-09-20 | 2011-04-06 | 中国海洋石油总公司 | Method for preparing special silica gel carrier with large pore volume and large specific surface area |
| CN102167337A (en) * | 2011-03-21 | 2011-08-31 | 冷水江三A化工有限责任公司 | Silicon dioxide aerogel and preparation method thereof |
| CN102199378A (en) * | 2011-03-21 | 2011-09-28 | 冷水江三A化工有限责任公司 | Preparation method for silica aerogel flatting agent |
| CN102145897A (en) * | 2011-04-19 | 2011-08-10 | 冷水江三A化工有限责任公司 | Large-pore-volume silicon dioxide with nanoparticle structure and preparation method thereof |
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