CN104276577B - A kind of have the precipitated silica of granule homogeneity, preparation method and its usage - Google Patents
A kind of have the precipitated silica of granule homogeneity, preparation method and its usage Download PDFInfo
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Abstract
A kind of method that the present invention relates to precipitated silica prepared and have granule homogeneity, it further relates in spherical microballon silicon dioxide and application thereof.Described silicon dioxide is characterised by that it contains: BET specific surface area is 100～250m2/g；Bulk density is 0.20～0.35cm3/g；Median D50At least 200 μm；40 mesh percent of pass >=90.0%, 120 mesh percent of pass≤12.0%；Free-running property≤35 °, moisture is≤7.0%.It is used as the carrier in feedstuff, pesticide, medicine and food service industry and anti-caking agent is used.
Description
Technical field
The present invention relates to the new method of a kind of precipitated silica prepared and there is granule homogeneity, further relate in
Spherical microballon silicon dioxide and powdered silica.
Background technology
Precipitated silica act as carrier and agglomeration resistance in the industries such as feedstuff, pesticide, medicine and food
Agent, is to flow freely the solid ingredient with storage-stable by liquid turns.
And use in the market at present a lot of be all powdery and superfine white carbon black, they in use stir
Time of mixing is long, poor mobile performance, and produces substantial amounts of powdery.
In order to reach by adding silicon dioxide acquisition optimum carrier and the purpose of agglomeration resistance effect, it is necessary to ensure that
The uniformity of silicon dioxide particle diameter, the hardness of granule and mobility, and in use without dust.
CN 1114832A discloses a kind of method preparing precipitated silica, including the silicon making a kind of alkali metal M
Hydrochlorate and a kind of acidulant react the suspension forming a kind of precipitated silica, are then peeled off and are dried above-mentioned suspension
Liquid, it is characterised in that precipitation is to carry out as got off: i) form a kind of silicic acid containing the alkali metal M for reaction
The mother solution of a part for the total amount of salt, in above-mentioned mother solution, the concentration (representing with SiO2) of silicate is less than 20g/l,
Ii) in above-mentioned mother solution, acidulant is added, until at least being present in above-mentioned starting stock solution of 5% quantity
M2O is neutralized, iii) in reaction medium, it is simultaneously introduced the silicic acid of the alkali metal M of acidulant and surplus
Salt so that the amount of the silicate of the amount (representing with SiO2) of the silicate of addition/be present in mother solution (uses SiO2
Represent) ratio (consolidation ratio) more than 4, but less than 100.
But prior art all cannot realize the preparation with the precipitated silica of granule homogeneity.
Summary of the invention
For the problem of prior art, the invention provides a kind of precipitation dioxy prepared and there is granule homogeneity
The new method of SiClx, use the precipitated silica that obtains of the method have granule uniformly, good flowing properties,
And the most non-dusting advantage.
To achieve these goals, present invention employs following technical scheme:
A kind of method preparing the precipitated silica with granule homogeneity, described method includes making waterglass
With concentrated sulphuric acid generation precipitation, thus obtain the suspension of precipitated silica, afterwards through filter pressing and wash
Wash, slurrying process be dried this suspension, wherein, carry out precipitation as follows:
(1) the preparation initial bed material of precipitation, wherein contains the waterglass used in described precipitation total
A part for amount, in described initial bed material, concentration of sodium silicate is with Na2O is expressed as 0.06～0.12N,
PH is 9.0～12.0；
(2) in described initial bed material, it is simultaneously added dropwise concentrated sulphuric acid and excess water glass, makes waterglass and concentrated sulphuric acid
There is precipitation；
(3) it is simultaneously added dropwise excess water glass and after concentrated sulphuric acid terminates, in reaction medium, individually drips dense sulfur
Acid；
Described filter pressing and washing process include that the silicon dioxide using membrane pressure filter to produce precipitation hangs
Filtration that supernatant liquid is carried out and washing operation, form the filter cake that solid content is more than 24wt%；
Described slurrying process includes that the filter cake using multi-stage stirrer and wet milk to produce filter pressing liquefies,
Forming silica suspension, the solid content of this suspension is more than 20wt%, and viscosity is
1000～2000cp.(the advantage that this solid content is high: (1) can reduce the energy consumption in dry run, reaches
Energy-conservation purpose, often improves the solid content of 1%, can energy efficient about 5%.(2) can ensure that bead particles
Intensity and homogeneity, and ensure do not crush).
Described dry run is through the suspension that pulp produces by pressure-type spray day with fog and is dried；
Described dry run also includes that dried product carries out redrying by fluid bed and separates with fine powder.
In the present invention, it is thus achieved that the essential condition of granule homogeneity silicon dioxide be pulp solid content and viscosity,
Drying mode and drying pressure.
Use membrane pressure filter to filter and wash, squeeze merit owing to the pressure filter of this structure has hydraulic pressure
Can, it can be ensured that obtained filter cake solid content is more than 24.0wt%.
The filter cake obtained after filtration washing carries out pulp by multi-stage stirrer and wet milk again, obtains solid content
Suspension for more than 20.0wt%.
Employing pressure type is dried, and is spherical microballon silicon dioxide with obtain.
Use fluid bed to carry out redrying in dry run to separate with fine powder, ensure silicon dioxide with this
Uniformity, mesh number percent of pass and the requirement of moisture.
In the present invention, step (1) first prepares the initial bed material of precipitation so that it is containing precipitation institute
A part for the waterglass total amount needed, is simultaneously added dropwise concentrated sulphuric acid and excess water glass the most wherein.
In step (1), described concentration of sodium silicate is with Na2O is expressed as 0.06～0.12N, such as 0.06N,
0.07N, 0.08N, 0.09N, 0.10N, 0.11N, 0.12N, preferably 0.06～0.08N.Described pH is
9.0～12.0, such as 9.0,10.0,11.0,12.0, preferably 9.0～11.0.
In the present invention, described concentrated sulphuric acid refers to the sulphuric acid that mass fraction is 98%.
In the present invention, the preparation raw material liq concentration of sodium silicate that used of the initial bed material of precipitation with
Na2O is expressed as 2.30～2.70N, such as 2.35,2.40,2.45,2.47,2.50,2.60, preferably
2.40～2.50N.
In the present invention, the time being simultaneously added dropwise concentrated sulphuric acid and excess water glass in step (2) is 60～150
Minute, such as 80 minutes, 90 minutes, 105 minutes, 120 minutes, 135 minutes.
In the present invention, controlling reaction temperature in step (2) is 75～95 DEG C, such as 75 DEG C, 80 DEG C,
85℃、90℃、95℃。
Additionally, during dripping concentrated sulphuric acid and excess water glass at the same time, remain that reaction temperature is constant
With the concentration of sodium silicate in reaction medium with Na2O be expressed as 0.06～0.12 (such as 0.06N, 0.07N,
0.10N, 0.12N) or pH be 6.0～12.0 (such as 9.0,9.5,10.0,10.5,11.0,11.5 steady
Fixed.
In the present invention, the concentration of described excess water glass is with Na2O is expressed as 2.30～2.70N, such as
2.35,2.40,2.45,2.47,2.50,2.60, preferably 2.40～2.50N.
Exemplary method is such as: first the present invention prepares the waterglass of above-mentioned concentration as raw material, uses this former
The initial bed material of reaction in material preparation steps (1), is then simultaneously added dropwise the above-mentioned of surplus in step (2) again
The waterglass of concentration.
After being simultaneously added dropwise concentrated sulphuric acid and excess water glass terminates, proceed by step (3).
In step (3), in reaction medium, individually drip concentrated sulphuric acid, to neutralize water remaining in reaction medium
Glass, the pH to reaction medium reaches 3.0～6.0, such as 3.2,3.5,4.0,4.5,5.0,5.5.
After step (3) terminates, it is thus achieved that silica suspension, then carry out filter pressing and washing.
In the present invention, membrane pressure filter is used to filter and wash, due to the filter pressing facility of this structure
There is water pressing function, it can be ensured that obtained filter cake solid content is more than 24.0wt%.
The filter cake obtained after filtration washing carries out pulp by multi-stage stirrer and wet milk again, obtains solid content
For the suspension of more than 20.0wt%, preferably 21.0～23.0wt%.
In the present invention, slurrying process can add appropriate additive, obtaining solid content be
21.0～23.0wt% and silica suspension that viscosity is 1000～2000cp.
Described dry run is through the suspension that pulp produces by pressure-type spray day with fog and is dried.
According to the present invention, be dried and use pressure type and be dried, it is thus achieved that be spherical microballon silicon dioxide,
Its median D50It is 200～300 μm.In dry run, the feed pressure being dried can pass through frequency conversion
Device regulates, common feed pressure 18～100bar, preferably 35～55bar.
Use fluid bed to carry out redrying in dry run to separate with fine powder, ensure silicon dioxide with this
Uniformity, mesh number percent of pass and the requirement of moisture.The median D of products obtained therefrom50At least
200 μm, preferably 200～280 μm；40 mesh percent of pass >=90.0%, preferably >=95%, 120 mesh percent of pass
≤ 12.0%, preferably≤10.0%；Product moisture is≤7.0%, preferably 4.0～5.0%.
The two of the purpose of the present invention are to provide a kind of and are had granule homogeneity by what method as defined above obtained
Precipitated silica, BET specific surface area is 100～250m2/ g, bulk density is 0.20～0.35cm3/ g, in
Position particle diameter D50 is at least 200 μm, 40 mesh percent of pass >=90.0%, 120 mesh percent of pass≤12.0%, scatters
Property≤35 °, moisture≤7.0%.
Preferably, BET specific surface area is 160～190m2/g。
Preferably, bulk density is 0.24～0.28cm3/g。
Preferably, median D50 is 200～300 μm.
Preferably, 40 mesh percent of pass >=95%.
Preferably, 120 mesh percent of pass≤10.0%
Preferably, free-running property≤25 °
Preferably, moisture is 4.0～5.0%.
The three of the purpose of the present invention are to provide a kind of precipitated silica as above with granule homogeneity
Silicon is as the carrier in feedstuff, pesticide, medicine and food service industry and the purposes of anti-caking agent.
Compared with the prior art, there is advantages that
The silicon dioxide that the present invention obtains, has granule uniform, and good flowing properties, in use without powder
Dirt, is widely used in the industries such as feedstuff, medicine, pesticide and food as carrier, anti-caking agent.
Detailed description of the invention
Technical scheme is further illustrated below by detailed description of the invention.
Embodiment 1
A kind of method preparing the precipitated silica with granule homogeneity, described method includes making waterglass
With concentrated sulphuric acid generation precipitation, thus obtain the suspension of precipitated silica, afterwards through filter pressing and wash
Wash, slurrying process be dried this suspension, wherein, carry out precipitation as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na2O table
It is shown as 2.35N
(2) use above-mentioned raw materials liquid soluble glass, prepare the initial bed material of precipitation, wherein contain described
The part of waterglass total amount used in precipitation, in described initial bed material, concentration of sodium silicate with
Na2It is 9.0 that O is expressed as 0.06N, pH；
(3) in 90 minutes, in described initial bed material, it is simultaneously added dropwise concentrated sulphuric acid and excess water glass, makes water
Glass and concentrated sulphuric acid generation precipitation, and to control reaction temperature be 75 DEG C, at the same time dropping concentrated sulphuric acid and remaining
During amount waterglass, remain that reaction temperature is constant and concentration of sodium silicate in reaction medium with
Na2It is 9.0 stablize that O is expressed as 0.06N or pH；
(4) it is simultaneously added dropwise excess water glass and after concentrated sulphuric acid terminates, in reaction medium, individually drips dense sulfur
Acid, the pH to reaction medium reaches 3.5；
Described filter pressing and washing process include that the silicon dioxide using membrane pressure filter to produce precipitation hangs
Filtration that supernatant liquid is carried out and washing operation, form the filter cake that solid content is more than 24wt%；
Described slurrying process includes that the filter cake using multi-stage stirrer and wet milk to produce filter pressing carries out fluid
Changing, form silica suspension, the solid content of this suspension is more than 22.0wt%, and viscosity is
1300cp；
Described dry run is through the suspension that pulp produces by pressure-type spray day with fog and is dried；
Described dry run also includes that dried product carries out redrying by fluid bed and separates with fine powder.
In dry run, the feed pressure being dried can be regulated by converter, common feed pressure
At 30bar.
Having the precipitated silica of granule homogeneity as above, BET specific surface area is 225m2/ g,
Bulk density is 0.245cm3/ g, median D50 are at least 310 μm, 40 mesh percent of pass 96.5%, and 120
Mesh percent of pass 4.8%, free-running property 24 °, moisture 5.6%.
Embodiment 2
A kind of method preparing the precipitated silica with granule homogeneity, described method includes making waterglass
With concentrated sulphuric acid generation precipitation, thus obtain the suspension of precipitated silica, afterwards through filter pressing and wash
Wash, slurrying process be dried this suspension, wherein, carry out precipitation as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na2O table
It is shown as 2.47N；
(2) the preparation initial bed material of precipitation, wherein contains the waterglass used in described precipitation total
A part for amount, in described initial bed material, concentration of sodium silicate is with Na2O is expressed as 0.07N, pH
10.0；
(3) in 120 minutes, in described initial bed material, it is simultaneously added dropwise concentrated sulphuric acid and excess water glass, makes water
Glass and concentrated sulphuric acid generation precipitation, and to control reaction temperature be 95 DEG C, at the same time dropping concentrated sulphuric acid and remaining
During amount waterglass, remain that reaction temperature is constant and concentration of sodium silicate in reaction medium with
Na2It is 10.0 stablize that O is expressed as 0.07N or pH；
(4) it is simultaneously added dropwise excess water glass and after concentrated sulphuric acid terminates, in reaction medium, individually drips dense sulfur
Acid, the pH to reaction medium reaches 4.0
Described filter pressing and washing process include that the silicon dioxide using membrane pressure filter to produce precipitation hangs
Filtration that supernatant liquid is carried out and washing operation, form the filter cake that solid content is more than 24wt%；
Described slurrying process includes that the filter cake using multi-stage stirrer and wet milk to produce filter pressing carries out fluid
Changing, form silica suspension, the solid content of this suspension is 21wt%, and viscosity is 1500cp；
Described dry run is through the suspension that pulp produces by pressure-type spray day with fog and is dried；
Described dry run also includes that dried product carries out redrying by fluid bed and separates with fine powder.
In dry run, the feed pressure being dried can be regulated by converter, common feed pressure
At 50bar.
Having the precipitated silica of granule homogeneity as above, BET specific surface area is 125m2/ g,
Bulk density is 0.253cm3/ g, median D50 are at least 285 μm, 40 mesh percent of pass 99.5%, and 120
Mesh percent of pass 6.5%, free-running property 18 °, moisture 4.6%.
Embodiment 3
A kind of method preparing the precipitated silica with granule homogeneity, described method includes making waterglass
With concentrated sulphuric acid generation precipitation, thus obtain the suspension of precipitated silica, afterwards through filter pressing and wash
Wash, slurrying process be dried this suspension, wherein, carry out precipitation as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na2O table
It is shown as 2.40N；
(2) the preparation initial bed material of precipitation, wherein contains the waterglass used in described precipitation total
A part for amount, in described initial bed material, concentration of sodium silicate is with Na2O is expressed as 0.10N, pH
10.5
(3) in 105 minutes, in described initial bed material, it is simultaneously added dropwise concentrated sulphuric acid and excess water glass, makes water
Glass and concentrated sulphuric acid generation precipitation, and to control reaction temperature be 80 DEG C, at the same time dropping concentrated sulphuric acid and remaining
During amount waterglass, remain that reaction temperature is constant and concentration of sodium silicate in reaction medium with
Na2It is 10.5 stablize that O is expressed as 0.10N or pH；
(4) it is simultaneously added dropwise excess water glass and after concentrated sulphuric acid terminates, in reaction medium, individually drips dense sulfur
Acid, the pH to reaction medium reaches 4.5；
Described filter pressing and washing process include that the silicon dioxide using membrane pressure filter to produce precipitation hangs
Filtration that supernatant liquid is carried out and washing operation, form the filter cake that solid content is more than 24wt%；
Described slurrying process includes that the filter cake using multi-stage stirrer and wet milk to produce filter pressing carries out fluid
Changing, form silica suspension, the solid content of this suspension is 23wt%, and viscosity is 1100cp；
Described dry run is through the suspension that pulp produces by pressure-type spray day with fog and is dried；
Described dry run also includes that dried product carries out redrying by fluid bed and separates with fine powder.
In dry run, the feed pressure being dried can be regulated by converter, common feed pressure
At 35bar.
Having the precipitated silica of granule homogeneity as above, BET specific surface area is 195m2/ g,
Bulk density is 0.258cm3/ g, median D50 are at least 300 μm, 40 mesh percent of pass 98.1%, and 120
Mesh percent of pass 6.8%, free-running property 20 °, moisture 4.6%.
Embodiment 4
A kind of method preparing the precipitated silica with granule homogeneity, described method includes making waterglass
With concentrated sulphuric acid generation precipitation, thus obtain the suspension of precipitated silica, afterwards through filter pressing and wash
Wash, slurrying process be dried this suspension, wherein, carry out precipitation as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na2O table
It is shown as 2.50N；
(2) the preparation initial bed material of precipitation, wherein contains the waterglass used in described precipitation total
A part for amount, in described initial bed material, concentration of sodium silicate is with Na2O is expressed as 0.12N, pH
For；11.5
(3) in 120 minutes, in described initial bed material, it is simultaneously added dropwise concentrated sulphuric acid and excess water glass, makes water
Glass and concentrated sulphuric acid generation precipitation, and to control reaction temperature be 85 DEG C, at the same time dropping concentrated sulphuric acid and remaining
During amount waterglass, remain that reaction temperature is constant and concentration of sodium silicate in reaction medium with
Na2It is 11.5 stablize that O is expressed as 0.12N or pH；
(4) it is simultaneously added dropwise excess water glass and after concentrated sulphuric acid terminates, in reaction medium, individually drips dense sulfur
Acid, the pH to reaction medium reaches 4；
Described filter pressing and washing process include that the silicon dioxide using membrane pressure filter to produce precipitation hangs
Filtration that supernatant liquid is carried out and washing operation, form the filter cake that solid content is more than 24wt%；
Described slurrying process includes that the filter cake using multi-stage stirrer and wet milk to produce filter pressing carries out fluid
Changing, form silica suspension, the solid content of this suspension is 22wt%, and viscosity is 1800Cp；
Described dry run is through the suspension that pulp produces by pressure-type spray day with fog and is dried；
Described dry run also includes that dried product carries out redrying by fluid bed and separates with fine powder.
In dry run, the feed pressure being dried can be regulated by converter, common feed pressure
For 55bar.
Having the precipitated silica of granule homogeneity as above, BET specific surface area is 176m2/ g,
Bulk density is 0.270cm3/ g, median D50 are at least 286 μm, 40 mesh percent of pass 99.1%, and 120
Mesh percent of pass 7.5%, free-running property 16 °, moisture 4.6%.
In above-described embodiment 1～4, alternatively, to obtain in addition to meeting solid content, viscosity is
The silica suspension of 1000～2000cp, adds additive in slurrying process.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the present invention
It is not limited to above-mentioned method detailed, does not i.e. mean that the present invention has to rely on above-mentioned method detailed ability real
Execute.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to product of the present invention
The equivalence of each raw material is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within the guarantor of the present invention
Within the scope of protecting scope and disclosure.
Claims (1)
1. the method preparing the precipitated silica with granule homogeneity, described method includes making water
Glass and concentrated sulphuric acid generation precipitation, thus obtain the suspension of precipitated silica, afterwards through filter pressing
And washing, slurrying process this suspension dry, wherein, carry out precipitation as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na2O table
It is shown as 2.35N；
(2) use above-mentioned raw materials liquid soluble glass, prepare the initial bed material of precipitation, wherein contain described
The part of waterglass total amount used in precipitation, in described initial bed material, concentration of sodium silicate with
Na2It is 9.0 that O is expressed as 0.06N, pH；
(3) in 90min, in described initial bed material, it is simultaneously added dropwise concentrated sulphuric acid and excess water glass, makes water glass
Glass and concentrated sulphuric acid generation precipitation, and to control reaction temperature be 75 DEG C, dropping concentrated sulphuric acid and surplus at the same time
During waterglass, remain that reaction temperature is constant and concentration of sodium silicate in reaction medium is with Na2O
Being expressed as 0.06N or pH is 9.0 stablize；
(4) it is simultaneously added dropwise excess water glass and after concentrated sulphuric acid terminates, in reaction medium, individually drips dense sulfur
Acid, the pH to reaction medium reaches 3.5；
Described filter pressing and washing process include that the silicon dioxide using membrane pressure filter to produce precipitation hangs
Filtration that supernatant liquid is carried out and washing operation, form the filter cake that solid content is more than 24wt%；
Described slurrying process includes that the filter cake using multi-stage stirrer and wet milk to produce filter pressing carries out fluid
Changing, form silica suspension, the solid content of this suspension is more than 22.0wt%, and viscosity is
1300cp；
Described dry run is that the suspension produced pulp by pressure-type spray day with fog is dried；
Described dry run also includes that dried product carries out redrying by fluid bed and separates with fine powder；
In dry run, the feed pressure being dried is regulated by converter, and feed pressure is at 30bar；
What described method prepared has the precipitated silica of granule homogeneity, and BET specific surface area is
225m2/ g, bulk density is 0.245g/cm3, median D50 is at least 310 μm, 40 mesh percent of pass
96.5%, 120 mesh percent of pass 4.8%, free-running property 24 °, moisture 5.6%.
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| CN109480097B (en) * | 2019-01-03 | 2022-02-01 | 山东联科科技股份有限公司 | Preparation method of silica microspheres for acidifier carrier |
| CN114349012B (en) * | 2022-01-21 | 2023-06-16 | 无锡恒诚硅业有限公司 | Preparation method and application of high-fluidity high-strength silicon dioxide |
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|---|---|---|---|---|
| CN1496959A (en) * | 1997-05-02 | 2004-05-19 | J.M. | Modified silicon dioxide product for elastomer |
| US20040161389A1 (en) * | 2003-02-14 | 2004-08-19 | J. M. Huber Corporation | Precipitated silica product with low surface area, dentifrices containing same, and processes |
| CN101774591A (en) * | 2010-02-26 | 2010-07-14 | 无锡恒诚硅业有限公司 | Production technology of white microsphere high-strength white carbon black |
| CN101830474A (en) * | 2010-05-17 | 2010-09-15 | 浙江建德建业有机化工有限公司 | Method for preparing white carbon black |
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2014
- 2014-09-22 CN CN201410488026.5A patent/CN104276577B/en active Active
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| CN1496959A (en) * | 1997-05-02 | 2004-05-19 | J.M. | Modified silicon dioxide product for elastomer |
| US20040161389A1 (en) * | 2003-02-14 | 2004-08-19 | J. M. Huber Corporation | Precipitated silica product with low surface area, dentifrices containing same, and processes |
| CN101774591A (en) * | 2010-02-26 | 2010-07-14 | 无锡恒诚硅业有限公司 | Production technology of white microsphere high-strength white carbon black |
| CN101830474A (en) * | 2010-05-17 | 2010-09-15 | 浙江建德建业有机化工有限公司 | Method for preparing white carbon black |
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