CN1418811A - Macroporous precipitation silicon dioxide used for achromatic colours, and its prepn. method - Google Patents
Macroporous precipitation silicon dioxide used for achromatic colours, and its prepn. method Download PDFInfo
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- CN1418811A CN1418811A CN 02156478 CN02156478A CN1418811A CN 1418811 A CN1418811 A CN 1418811A CN 02156478 CN02156478 CN 02156478 CN 02156478 A CN02156478 A CN 02156478A CN 1418811 A CN1418811 A CN 1418811A
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Abstract
The characteristics of silicon dioxide are: pore volume 0.4-1.8 cu.cm/g, BET specific surface area 130-350 sq.m/g, average pore size 180-300A, DBP value 2.0-4.0 ml/g, and grain size distribution D50 is 2.0-10.0 micrometer. Its preparation method includes the following steps: using alkaline silicate and acid as raw material and making them undergo the processes of precipitation reaction, ageing, filtering, washing, drying and pulverizing so as to obtain the invented large pore volume precipitate silicon dioxide product for delustering agent. It is characterized by that A, in the course of reaction adding water soluble surfactant, alcohol, organic amine salt or inorganic ammonium salt; and B in silicon dioxide suspension adding 1-5 g/L water soluble surfactant, alcohol, organic amine salt or inorganic ammonium salt, then spray-drying.
Description
Technical field
The invention belongs to technical field of powdered material preparation, particularly relate to a kind of matting agent large pore volume precipitated silica and preparation method thereof.
Background technology
Be used for coating the earliest, paint the fumed silica that is of making matting agent, but because it costs an arm and a leg, now precipitated gradually method silicon-dioxide replaces.At present, the operational path that the silicon-dioxide of the precipitator method (being wet method) preparation is both at home and abroad made matting agent mainly is divided into two classes: the first kind is a gel method, being about to certain density acid and alkali (alkaline silicate) reacts under acidity or alkaline condition, obtain the aqueous sol-gel of homogeneous, can obtain silica product through aging, fragmentation, washing, hydrothermal treatment consists, drying, pulverizing.(reference is seen US.6103,004; The open 8-170030 of special permission; Flat 9-30809; Flat 3-23211).The silica product that this method obtains has the structure height, and specific surface area is big, and pore volume is big, and pore size distribution is narrow and concentrated, also can keep the advantage of constructing under high shear forces, and have the good transparency; Shortcoming is that oil-absorption(number) is on the low side, technical process long, the last handling process energy consumption is big, causes product cost higher.The second class operational path is the precipitator method,, precipitin reaction is carried out in acid and alkaline silicate solution promptly under certain condition, the gel of silicic acid do not occur in the process and the SiO of loose, the flocks that obtains
2Particle, after filtration, washing, dry, pulverize and obtain silica product.The advantage of this method is a product oil-absorption(number) height, and processing condition are simple relatively, and cost is lower; Shortcoming is that products obtained therefrom is structural poor, and structure is easily destroyed under high-shear, and specific surface area is little, and pore volume is smaller (to be generally 0.6～1.0cm
3/ g), pore size distribution is wide, transparency difference etc.(reference is seen US.5123,964; US.5637,636; EP0341383 etc.).
Summary of the invention
The present invention provides a kind of matting agent large pore volume precipitated silica and preparation method thereof for solving the problem that known technology exists.
The precipitated silica that the purpose of this invention is to provide the large pore volume with certain specific character can be applicable to fields such as coating, rubber, printing ink, especially as the matting agent in the high-grade paint, and the characteristics that have high extinction, easily disperse, transparency are good.
The present invention adopts the precipitator method, has proposed a kind of processing method of special preparation precipitated silica.Concrete reactions steps of the present invention is: the first step, the alkali metal silicate solutions that accounts for total alkali content 10-50% is joined in the water of certain volume and be mixed with the dilute alkaline soln that volumetric molar concentration is 0.20-1.2M, then under 40-80 ℃ temperature to wherein adding acid solution, pH value until solution is 8.0-11.0, the pore structure control agent that adds 0.1～10.0% weight part, aging 10-30 minute; Second step was to be lower than under 100 ℃ of temperature of reaction, remaining alkali and acid are joined in the reaction mass within a certain period of time simultaneously, and the pH value of keeping reaction mass is 8.0～11.0; In the 3rd step, continuing acidifying is 4 until the pH value of reaction mass, keeps this temperature ageing 10～30 minutes then; It is good that the 4th step can obtain large pore volume, high oil-absorption(number) and the transparency with silica suspension filtration, washing, drying, pulverizing, and extinction is strong, easy dispersive silicon-dioxide.
Another characteristics of the present invention also are to have prepared a kind of silica flatting agent that coats with emulsifying wax.This kind matting agent is used for paint, coating, pigment, has the effect of easy dispersion, anti-settling.
The characteristic that precipitated silica provided by the invention has is:
Pore volume (ASAP2010) 0.4～1.8cm
3/ g is 1.4～1.6cm especially
3/ g
BET specific surface area 100～350m
2/ g 200～300m
2/ g
(nitrogen adsorption method, ASAP-2010 U.S. Micromertics company)
Mean pore size (ASAP2010) 150～300A 230～280 A
DBP value (HG/T 3072-1999) 2.0～4.0ml/g, 2.8～3.5ml/g
Size distribution 2.0～10.0 μ m (D50) 2.0～8.0 μ m
(accounting for more than 70% of all particles)
(laser granulometry, 100W ultrasonication 3 minutes)
Employed precipitation reactor is a stainless steel among the present invention, can carry out the steam jacket heating, and the agitator that uses can be turbine type, oblique oar formula and straight oar formula.
Employed alkali metal silicate solutions is water glass (SiO among the present invention
2: Na
2O=3.2～3.4: 1, SiO
2Content is 16.6%) (weight percent), (proportion is 1.1～1.84g/ml) for sulfuric acid in acid.
One of feature of the present invention is:
Can improve the pore structure of precipitated silica effectively by adding the pore structure control agent, the generation of small micelle in the inhibited reaction process reduces micro pore volume and obtains large pore volume (1.4～1.6cm
3/ g), pore size distribution 230～280A, specific surface area 200～350m
2The silica product of/g, oil-absorption(number) 2.8～3.5ml/g, median size 2.0～8.0.
Two of feature of the present invention is:
The pore structure control agent can be water miscible surface-modifying agent, comprises Sulfonates R-SO
3Na, phosphate ester salt R-OPO
3Na
2, sulfuric acid R-OSO
3Na, carboxylate salt R-COONa; Alcohol comprises glycerol, propyl carbinol, ethylene glycol etc.; Organic and inorganic amine comprises ammonia, volatile salt, bicarbonate of ammonia, ammonium sulfate, primary, the second month in a season, tertiary amine and quaternary ammonium salts.
Three of feature of the present invention:
In the silica suspension before carrying out spraying drying, pore structure control agent in the feature two of adding 1～5g/L, and then carry out spraying drying, also can increase the pore volume and the oil-absorption(number) of product effectively, but the specific surface area and the pore size distribution of product had certain influence.
Four of feature of the present invention:
A kind of preparation method of the precipitated silica that coats with emulsifying wax is provided.The silica product that this method obtains is compared with the silicon dioxide granule that coats without emulsifying wax, and is variant on physics, the chemical property.Weakened eliminate optical property to a certain extent, but it has anti-settling, make paint vehicle even, paint film is smooth to the touch, and does not produce the advantage of blue streak in surface of pigments, in addition, has shown that also its carbon content is 4～8%.The wax that can be used for preparing the wax emulsion has: polyethylene wax, Microcrystalline Wax, mineral wax, and composition thereof etc.Higher because of polyethylene wax zero pour and dropping point, emulsification condition and equipment requirements are higher.Obtained the good emulsifying effect so adopt the relatively low Microcrystalline Wax of zero pour (fusing point) to carry out emulsification among the present invention.
Five of feature of the present invention is:
The gained silicon dioxide granule is carried out superfine grinding, and classification, it is relatively concentrated to obtain size distribution, and particle size distribution accounts for more than 70～80% of product at the particle of 2～8 μ m.Because SiO
2The particle diameter of particle is meticulous, and less than 2 μ m, extinction is poor, if particle diameter is thick excessively, greater than 8 μ m, then influences the thickness and the slipperiness of paint film.
Matting agent of the present invention adopts following technical scheme with the large pore volume precipitated silica:
Matting agent large pore volume precipitated silica makes with alkaline silicate and Acid precipitation reaction, and its characteristic is: pore volume 0.4～1.8cm
3/ g, BET specific surface area 100～350m
2/ g, mean pore size 150～300A, DBP value 2.0～4.0ml/g, size distribution D50 are 2.0～10.0 μ m.
Matting agent of the present invention can also adopt following technical measures with the large pore volume precipitated silica:
Above-mentioned matting agent large pore volume precipitated silica is characterized in that pore volume is 1.4～1.6cm
3/ g.
Above-mentioned matting agent large pore volume precipitated silica is characterized in that the BET specific surface area is 200～300m
2/ g.
Above-mentioned matting agent large pore volume precipitated silica is characterized in that the DBP value is 2.8～3.5ml/g.
Above-mentioned matting agent large pore volume precipitated silica, its size distribution D50 are 2.0～8.0 μ m.
Matting agent of the present invention adopts following technical scheme with the preparation method of large pore volume precipitated silica:
The matting agent preparation method of large pore volume precipitated silica, with alkaline silicate and acid is that raw material carries out precipitin reaction, make through ageing, filtration, washing, drying, pulverizing then, be characterized in reaction process, adding water miscible surface-modifying agent, alcohol, organic amine salt or inorganic ammonium salt.
Matting agent of the present invention can also adopt following technical scheme with the preparation method of large pore volume precipitated silica:
The matting agent preparation method of large pore volume precipitated silica, with alkaline silicate and acid is that raw material carries out precipitin reaction, make through ageing, filtration, washing, drying, pulverizing then, be characterized in silica suspension, adding the water miscible surface-modifying agent of 1～5g/l, alcohol, organic amine salt or inorganic ammonium salt, and then carry out spraying drying.
Matting agent of the present invention can also adopt following technical measures with the preparation method of large pore volume precipitated silica:
Above-mentioned matting agent is characterized in using the emulsifying wax coated silica with the preparation method of large pore volume precipitated silica.
Above-mentioned matting agent is characterized in that with the preparation method of large pore volume precipitated silica water miscible surface-modifying agent is Sulfonates R-SO
3Na, phosphate ester salt R-OPO
3Na
2, sulfuric acid R-OSO
3Na, carboxylate salt R-COONa; Alcohol is glycerol, propyl carbinol, ethylene glycol; Organic amine salt is primary, secondary, tertiary amine and quaternary amine; Inorganic ammonium salt is volatile salt, bicarbonate of ammonia, ammonium sulfate.
The above-mentioned matting agent preparation method of large pore volume precipitated silica is characterized in:
(1) alkali metal silicate solutions that will account for total alkali content 10-50% adds and is mixed with the dilute alkaline soln that volumetric molar concentration is 0.2-1.2M in the entry, under 40-80 ℃ temperature, add acid then, pH value until solution is 8.0-11.0, the water-soluble surface-modifying agent, alcohol, organic amine salt or the inorganic ammonium salt that add 0.1～10.0% weight part, aging 10-30 minute;
(2) under 40～100 ℃ of temperature of reaction, remaining alkali and acid are joined in the reaction mass simultaneously, and the pH value of keeping reaction mass is 8.0～11.0;
(3) under 40～100 ℃ of temperature of reaction, continuing acidifying is 4 until the pH value of reaction mass, keeps this temperature ageing 10～30 minutes then;
(4) silica suspension filtration, washing, drying, pulverizing are made matting agent large pore volume precipitated silica.
Advantage that the present invention has and positively effect: the present invention is on the operational path of the precipitator method, selects for use special pore structure control agent can optionally regulate the size of pore volume in reaction process, has obtained well behaved silica product.This product had both had bigger pore volume and (can be 1.4～1.6cm
3/ g) and higher structure, and bigger specific surface area, pore size distribution concentrates, narrower, the characteristics that the transparency is good, this preparation method has overcome the shortcoming that the gel method technical process is long, cost is high, is suitable for commercial scale production, and good economic benefit is arranged.
Embodiment
For further understanding summary of the invention of the present invention, characteristics and effect, enumerate following example in detail now:
Embodiment 1
In the reactor of 5L belt stirrer, add 1000ml water, the 480ml sodium silicate solution stirs, and is warming up to 50 ℃, and under agitation the speed with 4ml/min drips d=1.20cm in solution
3The sulfuric acid of/g is 8～10 until the solution pH value, aging 30 minutes, continue to be warming up to 85 ℃, and under this temperature, in reactor, add water glass 820ml and sulfuric acid simultaneously, and maintenance solution pH value is 8～10.Reacting finishes continues to add acid to PH=4, with reaction paste ageing filtration in 15 minutes, washing, dry, pulverizing.
Embodiment 2
Method by example 1 narration prepares precipitated silica, and different with example 1 is:
Before the first step reaction is aging, add 10ml sodium dodecyl sulfate solution (100g/L).
Embodiment 3
By the method for example 1 narration prepare precipitated silica and example 1 different be:
Before in the first step reaction, wearing out, add 10ml butanol solution (1: 2).
Embodiment 4
Method by example 1 narration prepares precipitated silica, and with the silica filter cake that obtains after filtering, washing, reslurry is made aaerosol solution, and is to wherein adding 10ml sodium dodecyl sulfate solution (100g/L), dry then.
Embodiment 5
Method by example 2 narration prepares precipitated silica, with after filtration, the silica filter cake that obtains after the washing, reslurry is made suspension, to wherein adding 20ml wax emulsion, stirs that to make it chemical combination in 15 minutes even.
The preparation of wax emulsion can be carried out in the emulsor that has the high speed shear whipping appts.Get the Microcrystalline Wax (fusing point is 63～92 ℃) of 16.2 weight parts, add 3.8 weight part compound emulsifying agents, under about 100 ℃ temperature, make it fusing, under 80～90 ℃ condition, add the water of 80.0 weight parts then gradually.Make it to be converted into water, mixture is cooled to 60 ℃ then, finally obtain the emulsion of Microcrystalline Wax by oil phase.Test result is listed as follows:
Specific surface oil-absorption(number) pore volume mean pore size burning decrement size distribution
(m
2/g)?(ml/g) (cm
3/g)?(A) 1000℃2h 2～8μ
(%) m, (D50) mensuration of example 1 168 3.40 0.78 186 5.32 65 examples 2 276 3.52 1.64 238 4.15 72 examples 3 268 3.67 1.58 236 4.75 84 examples 4 233 3.60 1.47 252 6.24 76 examples 5 159 3.48 1.12 282 13.28 78 calcination alkali numbers is to carry out according to HG/T 3066-1999.
Claims (10)
1. matting agent large pore volume precipitated silica is to make with alkaline silicate and Acid precipitation reaction, it is characterized in that: pore volume 0.4～1.8cm
3/ g, BET specific surface area 100～350m
2/ g, mean pore size 150～300A, DBP value 2.0～4.0ml/g, size distribution D50 are 2.0～10.0 μ m.
2. matting agent large pore volume precipitated silica according to claim 1 is characterized in that: pore volume is 1.4～1.6cm
3/ g.
3. matting agent large pore volume precipitated silica according to claim 1 is characterized in that: the BET specific surface area is 200～300m
2/ g.
4. matting agent large pore volume precipitated silica according to claim 1 is characterized in that: the DBP value is 2.8～3.5ml/g.
5. matting agent large pore volume precipitated silica according to claim 1 is characterized in that: size distribution D50 is 2.0～8.0 μ m.
6. matting agent is with the preparation method of large pore volume precipitated silica, with alkaline silicate and acid is that raw material carries out precipitin reaction, make through ageing, filtration, washing, drying, pulverizing then, it is characterized in that: in reaction process, add water miscible surface-modifying agent, alcohol, organic amine salt or inorganic ammonium salt.
7. matting agent is with the preparation method of large pore volume precipitated silica, with alkaline silicate and acid is that raw material carries out precipitin reaction, make through ageing, filtration, washing, drying, pulverizing then, it is characterized in that: in silica suspension, add the water miscible surface-modifying agent of 1～5g/L, alcohol, organic amine salt or inorganic ammonium salt, and then carry out spraying drying.
8. according to the preparation method of claim 6 or 7 described matting agents usefulness large pore volume precipitated silicas, it is characterized in that: use the emulsifying wax coated silica.
9. according to the preparation method of claim 6 or 7 described matting agents usefulness large pore volume precipitated silicas, it is characterized in that: water miscible surface-modifying agent is Sulfonates R-SO
3Na, phosphate ester salt R-OPO
3Na
2, sulfuric acid R-OSO
3Na, carboxylate salt R-COONa; Alcohol is glycerol, propyl carbinol, ethylene glycol etc.; Organic amine salt is primary, secondary, tertiary amine and quaternary amine; Inorganic ammonium salt is ammonia, volatile salt, bicarbonate of ammonia, ammonium sulfate etc.
10. according to the preparation method of claim 6 or 7 described matting agents usefulness large pore volume precipitated silicas, it is characterized in that:
(1) alkali metal silicate solutions that will account for total alkali content 10-50% adds and is mixed with the dilute alkaline soln that volumetric molar concentration is 0.2-1.2M in the entry, under 40-80 ℃ temperature, add acid then, pH value until solution is 8.0-11.0, the water-soluble surface-modifying agent, alcohol, organic amine salt or the inorganic ammonium salt that add 0.1～10.0% weight part, aging 10-30 minute;
(2) under 40～100 ℃ of temperature of reaction, remaining alkali and acid are joined in the reaction mass simultaneously, and the pH value of keeping reaction mass is 8.0～11.0;
(3) under 40～100 ℃ of temperature of reaction, continuing acidifying is 4 until the pH value of reaction mass, keeps this temperature ageing 10～30 minutes then;
(4) silica suspension filtration, washing, drying, pulverizing are made matting agent large pore volume precipitated silica.
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| CN 02156478 CN1418811A (en) | 2002-12-18 | 2002-12-18 | Macroporous precipitation silicon dioxide used for achromatic colours, and its prepn. method |
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|---|---|---|---|
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| CN100572456C (en) * | 2006-04-24 | 2009-12-23 | 广州慧谷化学有限公司 | Nano inner core sandwich type structural silica dioxide delustring agent and preparation method thereof |
| CN101838479A (en) * | 2010-03-19 | 2010-09-22 | 福建师范大学 | Method for preparing dispersible ultra-fine silicon dioxide |
| CN101585540B (en) * | 2009-06-25 | 2011-01-05 | 福建省漳平市正盛化工有限公司 | Prepartion method of silicon dioxide with high pore volume |
| CN101948136A (en) * | 2010-09-13 | 2011-01-19 | 浙江工业大学 | Preparation method of laminated ammonium metatungstate with high dispersity |
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| US20220021077A1 (en) * | 2018-12-11 | 2022-01-20 | Rhodia Operations | Precipitated silica for battery separator |
| CN111470512A (en) * | 2019-03-13 | 2020-07-31 | 上海稷弘智能科技有限公司 | Method for preparing silica with high oil absorption value and large pore volume |
| CN110143599A (en) * | 2019-04-08 | 2019-08-20 | 杭州电子科技大学 | A kind of macropore appearance SiO2The novel preparation method of material |
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| CN112175432A (en) * | 2020-10-16 | 2021-01-05 | 北京航天赛德科技发展有限公司 | Composite anticorrosive pigment and preparation method and application thereof |
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