CN102199378A - Preparation method for silica aerogel flatting agent - Google Patents
Preparation method for silica aerogel flatting agent Download PDFInfo
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- CN102199378A CN102199378A CN2011100676699A CN201110067669A CN102199378A CN 102199378 A CN102199378 A CN 102199378A CN 2011100676699 A CN2011100676699 A CN 2011100676699A CN 201110067669 A CN201110067669 A CN 201110067669A CN 102199378 A CN102199378 A CN 102199378A
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Abstract
The invention relates to a preparation method for a silica aerogel flatting agent. The method comprises: adding 1-5% by weight of a retarding agent to alkaline silicate adopted as a raw material; adding an inorganic acid according to a weight ratio of the silica to the inorganic acid of 1:0.6, and carrying out a reaction for 1-5 hours at a temperature of 50-90 DEG C; adjusting pH value to 2-3; carrying out filtering and washing to obtain a filter cake having a sodium ion content below 0.1%; beating the filter cake through a high speed dispersing machine; heating to a temperature of 50-80 DEG C and adding a polyhydroxy compound to carry out a grafting reaction, wherein weight of the polyhydroxy compound is 1-2% of the weight of the alkaline silicate; then carrying out a drying process through a rapid dehydration, and carrying out a crushing process to obtain a finished product having a granularity of 3-9 [mu]m. The product prepared by the method provided by the present invention has a pore volume of 1.7-2.5 ml/g, a BET surface area of 300-400 m<2>/g, a silica content of 99.3% or more, a average granularity of 3-9 [mu]m, and good extinction performance. According to the present invention, compatibility with organic solvent is increased so as to provide a higher transparency and good recoatability for coating. The method has advantages of easy availability of the raw material, low price of the raw material, short process, and is easily applicable for realizing industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of aerosil matting agent.
Background technology
When the large aperture capacity silicon oxide aerogel uses as matting agent, its pore volume, specific surface area, mean particle size have very big influence to eliminate optical property, but because the distinctive hydrophilicity of silicon-dioxide itself, influenced its in paint organic solvent dispersiveness so that cause the properties of transparency of coating to descend the recoatability variation.The preparation of large aperture capacity silicon oxide mainly is a sol-gel method at present, owing to itself have the space three-dimensional reticulated structure, inside has been full of aperture, and the distribution of hydroxyl mainly is distributed in the inside in hole, makes itself and organic consistency variation, the transparency variation of coating.
Summary of the invention
The object of the present invention is to provide the preparation method of another kind of aerosil matting agent.To improve consistency and the dispersiveness of silicon-dioxide in coating.Make the transparency of coating higher, the recoat performance is good; And raw material is easy to get, and is cheap, and flow process is short, is easy to realize industrialization.
The preparation method of aerosil matting agent of the present invention may further comprise the steps:
(1) in the raw material alkaline silicate, adds the retardant calcium chloride of 1-5%, one or both the mixture in the magnesium chloride; According to silicon-dioxide: mineral acid weight ratio=1:0.6 adds mineral acid, under temperature 50-90 ℃, reacts 1-5 hour;
(2) adjust pH value 2-3 with mineral acid;
(3) reaction mass being filtered, is washed to sodium ions content is below 0.1%; And utilize high speed dispersor under 2000 rev/mins, filter cake is pulled an oar;
(4) with above-mentioned slurry heating, under temperature 50-80 ℃, the polyol that adds alkaline silicate weight 1-2% carried out graft reaction 1-2 hour, made wetting ability be converted to lipophilicity;
(5) under 100-400 ℃, carry out quick dewatering drying; It is the 3-9 micron that dried product is crushed to mean particle size.
Described alkaline silicate comprises one or both mixture of water glass, potassium silicate.
Described polyol comprises one or more of polyhydroxy fatty acid amide, hydroxycarboxylate and derivative thereof.
What described fast dewatering mode adopted is expansion drying or spraying drying.
The product pore volume that the present invention makes is 1.7-2.5ml/g, and the BET specific surface area is 300-400m
2/ g, dioxide-containing silica be more than 99.3%, mean particle size: 3-9 m; Eliminate optical property is good, the preparation method is that the employing alkaline silicate is that raw material adds retardant, the distribution of control silica sphere hydroxyl, adding polyol and silicon-dioxide carry out graft reaction and make wetting ability be converted to lipophilicity before dry, increased the consistency with organic solvent, made the coating transparency higher; The recoat performance is good; And raw material is easy, and is cheap, and flow process is short, is easy to realize industrialization.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1: make four parallel samples
The weight percent of getting silicon-dioxide is 10% sodium silicate solution 500g, adds 5g calcium chloride,
Add 20%(weight again) sulphuric acid soln 150g, 50 ℃ of temperature reaction 3 hours, adjusting pH value with sulfuric acid was 2-3; Filter cake after washing, will washing utilizes high speed dispersor under 2000 rev/mins again, and filter cake is pulled an oar; Above-mentioned slurry is heated to 50 ℃, adds polyhydroxy fatty acid amide 0.5g, reacted 2 hours.Spraying drying and size classification mean particle size 3-5 micron obtain the polymolecularity aerosil.Its physical and chemical performance is as follows
Embodiment 1: polymolecularity aerosil physical and chemical performance table
Embodiment 2: make four parallel samples
Getting dioxide-containing silica is 15%(weight) sodium silicate solution 500g.Add 0.75 magnesium chloride, add 10% sulfuric acid (weight) solution 450g again; 50 ℃ of reactions of temperature 5 hours, the adjustment pH value was 2-3; Leave standstill processing by prior art through wearing out.Again after filtration, washing and utilize high speed dispersor under 2000 rev/mins, filter cake is pulled an oar, above-mentioned slurry is heated to 70 ℃, add 0.75g hydroxycarboxylate and derivative thereof, be incubated 2 hours.Spraying drying and pulverizing obtain mean particle size 5-9 micron polymolecularity aerosil.Its experimental data is as follows.
Embodiment 2: polymolecularity aerosil physical and chemical performance table
Embodiment 3: make four parallel samples
Getting dioxide-containing silica is the sodium silicate solution 500g of 12% (weight); Sulfuric acid (weight) the solution 180g that adds 0.6g magnesium chloride and 20%; 70 ℃ of reactions of temperature 5 hours, adding acid adjustment pH value was 2-3; Leave standstill processing by prior art through wearing out.Again after filtration, the washing, filter cake is pulled an oar under 2000 rev/mins with high speed dispersor, above-mentioned slurry is heated to 70 ℃, the adding polyhydroxy fatty acid amide, hydroxycarboxylate and each 0.6g of derivative thereof, be incubated 2 hours.Spraying drying and pulverizing obtain mean particle size 6-8 micron, obtain the polymolecularity aerosil.Its experimental data is as follows
Embodiment 3: polymolecularity aerosil physical and chemical performance table
Claims (4)
1. the preparation method of an aerosil matting agent is characterized in that, may further comprise the steps:
(1) in the raw material alkaline silicate, adds the retardant calcium chloride of 1-5%, one or both the mixture in the magnesium chloride; According to silicon-dioxide: mineral acid weight ratio=1:0.6 adds mineral acid, under temperature 50-90 ℃, reacts 1-5 hour;
(2) adjust pH value 2-3 with mineral acid;
(3) reaction mass being filtered, is washed to sodium ions content is below 0.1%; And utilize high speed dispersor under 2000 rev/mins, filter cake is pulled an oar;
(4) with above-mentioned slurry heating, under temperature 50-80 ℃, the polyol that adds alkaline silicate weight 1-2% carried out graft reaction 1-2 hour, made wetting ability be converted to lipophilicity;
(6) under 100-400 ℃, carry out quick dewatering drying; It is the 3-9 micron that dried product is crushed to mean particle size.
2. the preparation method of aerosil matting agent according to claim 1 is characterized in that, described alkaline silicate comprises one or both mixture of water glass, potassium silicate.
3. the preparation method of aerosil matting agent according to claim 1 is characterized in that, described polyol comprises one or more of polyhydroxy fatty acid amide, hydroxycarboxylate and derivative thereof.
4. the preparation method of aerosil matting agent according to claim 1 is characterized in that, what described fast dewatering mode adopted is expansion drying or spraying drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100676699A CN102199378A (en) | 2011-03-21 | 2011-03-21 | Preparation method for silica aerogel flatting agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100676699A CN102199378A (en) | 2011-03-21 | 2011-03-21 | Preparation method for silica aerogel flatting agent |
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| CN102199378A true CN102199378A (en) | 2011-09-28 |
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| CN2011100676699A Pending CN102199378A (en) | 2011-03-21 | 2011-03-21 | Preparation method for silica aerogel flatting agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530970A (en) * | 2012-03-01 | 2012-07-04 | 冷水江三A化工有限责任公司 | Preparation method of toothpaste abrasive silicon dioxide |
| CN103785350A (en) * | 2014-01-08 | 2014-05-14 | 冷水江三A化工有限责任公司 | Preparation method of silicon dioxide cationic adsorbent |
| CN104530770A (en) * | 2015-01-26 | 2015-04-22 | 广东海顺新材料科技有限公司 | Preparation method of high-transparency low-oil-absorption-number matting powder |
| CN112408400A (en) * | 2020-11-04 | 2021-02-26 | 福建中闽大地纳米新材料有限公司 | Water-saving and energy-saving precipitation production method of silicon dioxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0442325A1 (en) * | 1990-02-14 | 1991-08-21 | Grace GmbH | Si02-Flatting agent, process for its production and its use |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN101274762A (en) * | 2007-03-29 | 2008-10-01 | 北京市华从经贸有限责任公司 | Modification method for silicon dioxide aerogel |
| CN101407324A (en) * | 2008-06-02 | 2009-04-15 | 通化双龙化工股份有限公司 | Method of preparing silicon dioxide delustrant by large pore volume gel |
-
2011
- 2011-03-21 CN CN2011100676699A patent/CN102199378A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0442325A1 (en) * | 1990-02-14 | 1991-08-21 | Grace GmbH | Si02-Flatting agent, process for its production and its use |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN101274762A (en) * | 2007-03-29 | 2008-10-01 | 北京市华从经贸有限责任公司 | Modification method for silicon dioxide aerogel |
| CN101407324A (en) * | 2008-06-02 | 2009-04-15 | 通化双龙化工股份有限公司 | Method of preparing silicon dioxide delustrant by large pore volume gel |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530970A (en) * | 2012-03-01 | 2012-07-04 | 冷水江三A化工有限责任公司 | Preparation method of toothpaste abrasive silicon dioxide |
| CN102530970B (en) * | 2012-03-01 | 2014-02-19 | 冷水江三A化工有限责任公司 | Preparation method of toothpaste abrasive silicon dioxide |
| CN103785350A (en) * | 2014-01-08 | 2014-05-14 | 冷水江三A化工有限责任公司 | Preparation method of silicon dioxide cationic adsorbent |
| CN103785350B (en) * | 2014-01-08 | 2015-07-08 | 冷水江三A新材料科技有限公司 | Preparation method of silicon dioxide cationic adsorbent |
| CN104530770A (en) * | 2015-01-26 | 2015-04-22 | 广东海顺新材料科技有限公司 | Preparation method of high-transparency low-oil-absorption-number matting powder |
| CN104530770B (en) * | 2015-01-26 | 2016-03-30 | 广东海顺新材料科技有限公司 | The preparation method of the low oil-absorption(number) flatting silica of a kind of high transparency |
| CN112408400A (en) * | 2020-11-04 | 2021-02-26 | 福建中闽大地纳米新材料有限公司 | Water-saving and energy-saving precipitation production method of silicon dioxide |
| CN112408400B (en) * | 2020-11-04 | 2022-07-26 | 福建中闽大地纳米新材料有限公司 | Water-saving and energy-saving precipitation production method of silicon dioxide |
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Application publication date: 20110928 |