CN104276577A - Precipitated silicon dioxide with particle uniformity, preparation method and use of precipitated silicon dioxide - Google Patents
Precipitated silicon dioxide with particle uniformity, preparation method and use of precipitated silicon dioxide Download PDFInfo
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- CN104276577A CN104276577A CN201410488026.5A CN201410488026A CN104276577A CN 104276577 A CN104276577 A CN 104276577A CN 201410488026 A CN201410488026 A CN 201410488026A CN 104276577 A CN104276577 A CN 104276577A
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Abstract
The invention relates to a method for preparing precipitated silicon dioxide with particle uniformity and further relates to spherical microbead silicon dioxide and use thereof. The silicon dioxide has the characteristics that the BET specific surface area is 100-250m<2>/g; the bulk density is 0.20-0.35cm<3>/g; the median particle diameter D50 is at least 200 mu m; the 40-mesh passing rate is greater than or equal to 90.0%; the 120-mesh passing rate is less than or equal to 12.0%; the free-running property is less than or equal to 35 degrees; the moisture is less than or equal to 7.0%. The precipitated silicon dioxide is used as a carrier and an anticaking agent in the industries of feeds, pesticides, medicines and foods.
Description
Technical field
The present invention relates to a kind of novel method preparing the precipitated silica with particle homogeneity, also relate in spherical microballon silicon-dioxide and powdered silica.
Background technology
Precipitated silica act as carrier and anti-caking agent in the industries such as feed, agricultural chemicals, medicine and food, is can the solid ingredient of unrestricted flow and stably stored by liquid turns.
And use in the market at present a lot of be all powdery and superfine white carbon black, in use churning time is long for they, poor mobile performance, and produces a large amount of powderies.
Adding to be reached through the object that silicon-dioxide obtains optimum carrier and agglomeration resistance effect, the homogeneity of silicon-dioxide particle diameter, the hardness of particle and mobility must be guaranteed, and in use without dust.
CN 1114832A discloses a kind of method preparing precipitated silica, comprise and make the silicate of a kind of basic metal M and a kind of souring agent react the suspension forming a kind of precipitated silica, then be separated and dry above-mentioned suspension, it is characterized in that precipitation is carried out as follows: mother liquor i) forming an a kind of part of total amount of the silicate containing the basic metal M for reacting, the concentration (representing with SiO2) of above-mentioned mother liquor mesosilicic acid salt is lower than 20g/l, ii) in above-mentioned mother liquor, souring agent is added, until have the M be present in above-mentioned starting stock solution of 5% quantity at least
2o is neutralized, iii) in reaction medium, add the silicate of the basic metal M of souring agent and residual content simultaneously, make the ratio (consolidation ratio) of the amount of the silicate added (representing with SiO2)/the be present in amount (representing with SiO2) of the silicate in mother liquor be greater than 4, but be no more than 100.
But prior art all cannot realize the preparation of the precipitated silica with particle homogeneity.
Summary of the invention
For the problem of prior art, the invention provides a kind of novel method preparing the precipitated silica with particle homogeneity, adopt the precipitated silica that obtains of the method to have uniform particles, good flowing properties and in use non-dusting advantage.
To achieve these goals, present invention employs following technical scheme:
A kind of method preparing the precipitated silica with particle homogeneity, described method comprises makes water glass and vitriol oil generation precipitin reaction, thus obtain the suspension of precipitated silica, afterwards through press filtration and washing, slurrying process this suspension dry, wherein, precipitin reaction is carried out as follows:
(1) prepare the initial bed material of precipitin reaction, the part wherein containing the water glass total amount used in described precipitin reaction, in described initial bed material, concentration of sodium silicate is with Na
2o is expressed as 0.06 ~ 0.12N, and pH is 9.0 ~ 12.0;
(2) in described initial bed material, drip the vitriol oil and excess water glass simultaneously, make water glass and vitriol oil generation precipitin reaction;
(3), after dropping excess water glass and the vitriol oil terminate simultaneously, in reaction medium, the vitriol oil is dripped separately;
Described press filtration and washing process comprise the filtration and washing operation that adopt membrane pressure filter to carry out the silica suspension that precipitin reaction is produced, and formation solid content is the filter cake of more than 24wt%;
Described slurrying process comprises employing multi-stage stirrer and wet wheeling machine liquefies to the filter cake that press filtration produces, and form silica suspension, the solid content of this suspension is more than 20wt%, and viscosity is 1000 ~ 2000cp.(advantage that this solid content is high: (1) can reduce the energy consumption in drying process, reaches energy-conservation object, often improves the solid content of 1%, can energy efficient about 5%.(2) intensity and the homogeneity of bead particles can be guaranteed, and ensure in use not broken).
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces;
Described drying process also comprises dried product and carries out redrying by fluidized-bed and be separated with fine powder.
In the present invention, the essential condition obtaining particle homogeneity silicon-dioxide is pulp solid content and viscosity, drying mode and drying pressure.
Adopt membrane pressure filter to carry out filtering and washing, the pressure filter due to this structure has water pressing function, can guarantee 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 wheeling machine again, obtains the suspension that solid content is more than 20.0wt%.
Employing pressure type is dry, is spherical microballon silicon-dioxide with what obtain.
In drying process, adopt fluidized-bed to carry out redrying be separated with fine powder, ensure the requirement of the homogeneity of silicon-dioxide, order number percent of pass and moisture with this.
In the present invention, step (1) first prepares the initial bed material of precipitin reaction, makes it contain a part for the water glass total amount required for precipitin reaction, and then drips the vitriol oil and excess water glass wherein simultaneously.
In step (1), described concentration of sodium silicate is with Na
2o 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, the described vitriol oil refers to that massfraction is the sulfuric acid of 98%.
In the present invention, raw material liq concentration of sodium silicate that precipitin reaction initial bed material uses is prepared with Na
2o is expressed as 2.30 ~ 2.70N, and 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 simultaneously dripping the vitriol oil and excess water glass in step (2) is 60 ~ 150 minutes, such as 80 minutes, 90 minutes, 105 minutes, 120 minutes, 135 minutes.
In the present invention, controlling temperature of reaction in step (2) is 75 ~ 95 DEG C, such as 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C.
In addition, drip at the same time in the process of the vitriol oil and excess water glass, remain that concentration of sodium silicate in the constant and reaction medium of temperature of reaction is with Na
2it is 6.0 ~ 12.0 (such as 9.0,9.5,10.0,10.5,11.0,11.5 stablize that O is expressed as 0.06 ~ 0.12 (such as 0.06N, 0.07N, 0.10N, 0.12N) or pH.
In the present invention, the concentration of described excess water glass is with Na
2o is expressed as 2.30 ~ 2.70N, and such as 2.35,2.40,2.45,2.47,2.50,2.60, preferably 2.40 ~ 2.50N.
Exemplary method as: first the present invention prepares the water glass of above-mentioned concentration as raw material, adopts the initial bed material of reaction in this preparation of raw material step (1), then drips the water glass of the above-mentioned concentration of surplus in step (2) more simultaneously.
After dripping the vitriol oil and excess water glass simultaneously and terminating, start to carry out step (3).
In step (3), in reaction medium, drip the vitriol oil separately, with water glass remaining in neutralization reaction medium, the pH to reaction medium reaches 3.0 ~ 6.0, and such as 3.2,3.5,4.0,4.5,5.0,5.5.
After step (3) terminates, obtain silica suspension, then carry out press filtration and washing.
In the present invention, adopt membrane pressure filter to carry out filtering and washing, the pressure filter due to this structure has water pressing function, can guarantee 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 wheeling machine again, obtains the suspension that solid content is more than 20.0wt%, preferably 21.0 ~ 23.0wt%.
In the present invention, can add appropriate additive in slurrying process, be the silica suspension of 1000 ~ 2000cp to obtain solid content be 21.0 ~ 23.0wt% and viscosity.
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces.
According to the present invention, dry what adopt is that pressure type is dry, acquisition be spherical microballon silicon-dioxide, its median D
50it is 200 ~ 300 μm.In drying process, dry feed pressure can be regulated by frequency transformer, common feed pressure at 18 ~ 100bar, preferably 35 ~ 55bar.
In drying process, adopt fluidized-bed to carry out redrying be separated with fine powder, ensure the requirement of the homogeneity of silicon-dioxide, order number percent of pass and moisture with this.The median D of products obtained therefrom
50be at least 200 μm, be preferably 200 ~ 280 μm; 40 order percent of pass>=90.0%, preferably>=95%, 120 order percent of pass≤12.0%, preferably≤10.0%; Product moisture is≤7.0%, preferably 4.0 ~ 5.0%.
Two of object of the present invention is to provide a kind of precipitated silica with particle homogeneity obtained by method described above, and BET specific surface area is 100 ~ 250m
2/ g, tap density is 0.20 ~ 0.35cm
3/ g, median D50 is at least 200 μm, 40 order percent of pass>=90.0%, 120 order percent of pass≤12.0%, free-running property≤35 °, moisture≤7.0%.
Preferably, BET specific surface area is 160 ~ 190m
2/ g.
Preferably, tap density is 0.24 ~ 0.28cm
3/ g.
Preferably, median D50 is 200 ~ 300 μm.
Preferably, 40 order percent of pass >=95%.
Preferably, 120 order percent of pass≤10.0%
Preferably, free-running property≤25 °
Preferably, moisture is 4.0 ~ 5.0%.
Three of object of the present invention is to provide a kind of precipitated silica as above with particle homogeneity as the purposes of the carrier in feed, agricultural chemicals, medicine and food service industry and anti-caking agent.
Compared with the prior art, the present invention has following beneficial effect:
The silicon-dioxide that the present invention obtains, has uniform particles, good flowing properties, in use without dust, is widely used in the industries such as feed, medicine, agricultural chemicals and food as carrier, anti-caking agent.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.
Embodiment 1
A kind of method preparing the precipitated silica with particle homogeneity, described method comprises makes water glass and vitriol oil generation precipitin reaction, thus obtain the suspension of precipitated silica, afterwards through press filtration and washing, slurrying process this suspension dry, wherein, precipitin reaction is carried out as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na
2o is expressed as 2.35N
(2) adopt above-mentioned raw materials liquid soluble glass, the initial bed material of preparation precipitin reaction, the part wherein containing the water glass total amount used in described precipitin reaction, in described initial bed material, concentration of sodium silicate is with Na
2o is expressed as 0.06N, and pH is 9.0;
(3) in 90 minutes, in described initial bed material, drip the vitriol oil and excess water glass simultaneously, make water glass and vitriol oil generation precipitin reaction, and to control temperature of reaction be 75 DEG C, drip in the process of the vitriol oil and excess water glass at the same time, remain that concentration of sodium silicate in the constant and reaction medium of temperature of reaction is with Na
2o be expressed as 0.06N or pH be 9.0 stable;
(4), after dropping excess water glass and the vitriol oil terminate simultaneously, in reaction medium, drip the vitriol oil separately, the pH to reaction medium reaches 3.5;
Described press filtration and washing process comprise the filtration and washing operation that adopt membrane pressure filter to carry out the silica suspension that precipitin reaction is produced, and formation solid content is the filter cake of more than 24wt%;
Described slurrying process comprises employing multi-stage stirrer and wet wheeling machine carries out fluidization to the filter cake that press filtration produces, and form silica suspension, the solid content of this suspension is more than 22.0wt%, and viscosity is 1300cp;
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces;
Described drying process also comprises dried product and carries out redrying by fluidized-bed and be separated with fine powder.
In drying process, dry feed pressure can be regulated by frequency transformer, and common feed pressure is at 30bar.
Have the precipitated silica of particle homogeneity as above, BET specific surface area is 225m
2/ g, tap density is 0.245cm
3/ g, median D50 is at least 310 μm, 40 order percent of pass 96.5%, 120 order percent of pass 4.8%, free-running property 24 °, moisture 5.6%.
Embodiment 2
A kind of method preparing the precipitated silica with particle homogeneity, described method comprises makes water glass and vitriol oil generation precipitin reaction, thus obtain the suspension of precipitated silica, afterwards through press filtration and washing, slurrying process this suspension dry, wherein, precipitin reaction is carried out as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na
2o is expressed as 2.47N;
(2) prepare the initial bed material of precipitin reaction, the part wherein containing the water glass total amount used in described precipitin reaction, in described initial bed material, concentration of sodium silicate is with Na
2o is expressed as 0.07N, and pH is 10.0;
(3) in 120 minutes, in described initial bed material, drip the vitriol oil and excess water glass simultaneously, make water glass and vitriol oil generation precipitin reaction, and to control temperature of reaction be 95 DEG C, drip in the process of the vitriol oil and excess water glass at the same time, remain that concentration of sodium silicate in the constant and reaction medium of temperature of reaction is with Na
2o be expressed as 0.07N or pH be 10.0 stable;
(4), after dropping excess water glass and the vitriol oil terminate simultaneously, in reaction medium, drip the vitriol oil separately, the pH to reaction medium reaches 4.0
Described press filtration and washing process comprise the filtration and washing operation that adopt membrane pressure filter to carry out the silica suspension that precipitin reaction is produced, and formation solid content is the filter cake of more than 24wt%;
Described slurrying process comprises employing multi-stage stirrer and wet wheeling machine carries out fluidization to the filter cake that press filtration produces, and form silica suspension, the solid content of this suspension is 21wt%, and viscosity is 1500cp;
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces;
Described drying process also comprises dried product and carries out redrying by fluidized-bed and be separated with fine powder.
In drying process, dry feed pressure can be regulated by frequency transformer, and common feed pressure is at 50bar.
Have the precipitated silica of particle homogeneity as above, BET specific surface area is 125m
2/ g, tap density is 0.253cm
3/ g, median D50 is at least 285 μm, 40 order percent of pass 99.5%, 120 order percent of pass 6.5%, free-running property 18 °, moisture 4.6%.
Embodiment 3
A kind of method preparing the precipitated silica with particle homogeneity, described method comprises makes water glass and vitriol oil generation precipitin reaction, thus obtain the suspension of precipitated silica, afterwards through press filtration and washing, slurrying process this suspension dry, wherein, precipitin reaction is carried out as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na
2o is expressed as 2.40N;
(2) prepare the initial bed material of precipitin reaction, the part wherein containing the water glass total amount used in described precipitin reaction, in described initial bed material, concentration of sodium silicate is with Na
2o is expressed as 0.10N, and pH is 10.5
(3) in 105 minutes, in described initial bed material, drip the vitriol oil and excess water glass simultaneously, make water glass and vitriol oil generation precipitin reaction, and to control temperature of reaction be 80 DEG C, drip in the process of the vitriol oil and excess water glass at the same time, remain that concentration of sodium silicate in the constant and reaction medium of temperature of reaction is with Na
2o be expressed as 0.10N or pH be 10.5 stable;
(4), after dropping excess water glass and the vitriol oil terminate simultaneously, in reaction medium, drip the vitriol oil separately, the pH to reaction medium reaches 4.5;
Described press filtration and washing process comprise the filtration and washing operation that adopt membrane pressure filter to carry out the silica suspension that precipitin reaction is produced, and formation solid content is the filter cake of more than 24wt%;
Described slurrying process comprises employing multi-stage stirrer and wet wheeling machine carries out fluidization to the filter cake that press filtration produces, and form silica suspension, the solid content of this suspension is 23wt%, and viscosity is 1100cp;
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces;
Described drying process also comprises dried product and carries out redrying by fluidized-bed and be separated with fine powder.
In drying process, dry feed pressure can be regulated by frequency transformer, and common feed pressure is at 35bar.
Have the precipitated silica of particle homogeneity as above, BET specific surface area is 195m
2/ g, tap density is 0.258cm
3/ g, median D50 is at least 300 μm, 40 order percent of pass 98.1%, 120 order percent of pass 6.8%, free-running property 20 °, moisture 4.6%.
Embodiment 4
A kind of method preparing the precipitated silica with particle homogeneity, described method comprises makes water glass and vitriol oil generation precipitin reaction, thus obtain the suspension of precipitated silica, afterwards through press filtration and washing, slurrying process this suspension dry, wherein, precipitin reaction is carried out as follows:
(1) preparation raw material liquid soluble glass, in described liquid soluble glass, concentration of sodium silicate is with Na
2o is expressed as 2.50N;
(2) prepare the initial bed material of precipitin reaction, the part wherein containing the water glass total amount used in described precipitin reaction, in described initial bed material, concentration of sodium silicate is with Na
2o is expressed as 0.12N, and pH is; 11.5
(3) in 120 minutes, in described initial bed material, drip the vitriol oil and excess water glass simultaneously, make water glass and vitriol oil generation precipitin reaction, and to control temperature of reaction be 85 DEG C, drip in the process of the vitriol oil and excess water glass at the same time, remain that concentration of sodium silicate in the constant and reaction medium of temperature of reaction is with Na
2o be expressed as 0.12N or pH be 11.5 stable;
(4), after dropping excess water glass and the vitriol oil terminate simultaneously, in reaction medium, drip the vitriol oil separately, the pH to reaction medium reaches 4;
Described press filtration and washing process comprise the filtration and washing operation that adopt membrane pressure filter to carry out the silica suspension that precipitin reaction is produced, and formation solid content is the filter cake of more than 24wt%;
Described slurrying process comprises employing multi-stage stirrer and wet wheeling machine carries out fluidization to the filter cake that press filtration produces, and form silica suspension, the solid content of this suspension is 22wt%, and viscosity is 1800Cp;
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces;
Described drying process also comprises dried product and carries out redrying by fluidized-bed and be separated with fine powder.
In drying process, dry feed pressure can be regulated by frequency transformer, and common feed pressure is 55bar.
Have the precipitated silica of particle homogeneity as above, BET specific surface area is 176m
2/ g, tap density is 0.270cm
3/ g, median D50 is at least 286 μm, 40 order percent of pass 99.1%, 120 order percent of pass 7.5%, free-running property 16 °, moisture 4.6%.
In above-described embodiment 1 ~ 4, alternatively, to obtain except meeting solid content, viscosity is the silica suspension of 1000 ~ 2000cp, in slurrying process, add additive.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. prepare the method for the precipitated silica with particle homogeneity for one kind, described method comprises makes water glass and vitriol oil generation precipitin reaction, thus obtain the suspension of precipitated silica, afterwards through press filtration and washing, slurrying process this suspension dry, wherein, precipitin reaction is carried out as follows:
(1) prepare the initial bed material of precipitin reaction, the part wherein containing the water glass total amount used in described precipitin reaction, in described initial bed material, concentration of sodium silicate is with Na
2o is expressed as 0.06 ~ 0.12N, and pH is 9.0 ~ 12.0;
(2) in described initial bed material, drip the vitriol oil and excess water glass simultaneously, make water glass and vitriol oil generation precipitin reaction;
(3), after dropping excess water glass and the vitriol oil terminate simultaneously, in reaction medium, the vitriol oil is dripped separately;
Described press filtration and washing process comprise the filtration and washing operation that adopt membrane pressure filter to carry out the silica suspension that precipitin reaction is produced, and formation solid content is the filter cake of more than 24wt%;
Described slurrying process comprises employing multi-stage stirrer and wet wheeling machine liquefies to the filter cake that press filtration produces, and form silica suspension, the solid content of this suspension is more than 20wt%, and viscosity is 1000 ~ 2000cp;
Described drying process is exactly carry out drying by pressure-type spray day with fog to the suspension that pulp produces;
Described drying process also comprises dried product and carries out redrying by fluidized-bed and be separated with fine powder.
2. the method for claim 1, is characterized in that, the raw material liq concentration of sodium silicate that the initial bed material of preparation precipitin reaction uses is with Na
2o is expressed as 2.30 ~ 2.70N, preferably 2.40 ~ 2.50N;
Preferably, the time simultaneously dripping the vitriol oil and excess water glass in step (2) is 60 ~ 150 minutes;
Preferably, controlling temperature of reaction in step (2) is 75 ~ 95 DEG C.
3. method as claimed in claim 1 or 2, is characterized in that, drips at the same time in the process of the vitriol oil and excess water glass, remains that concentration of sodium silicate in the constant and reaction medium of temperature of reaction is with Na
2o be expressed as 0.06 ~ 0.12N or pH be 9.0 ~ 12.0 stable;
Preferably, the concentration of described excess water glass is with Na
2o is expressed as 2.30 ~ 2.70N.
4. the method as described in one of claim 1-3, is characterized in that, in reaction medium, drip the vitriol oil separately, and the pH to reaction medium reaches 3.0 ~ 6.0.
5. the method as described in one of claim 1-4, is characterized in that, the solid content of the silica suspension that pulp obtains is 21.0 ~ 23.0wt%;
Preferably, in slurrying process, adding additive, is the silica suspension of 1000 ~ 2000cp to obtain solid content be 21.0 ~ 23.0wt% and viscosity.
6. the method as described in one of claim 1-5, is characterized in that, in drying process, dry feed pressure is regulated by frequency transformer, and feed pressure is 18 ~ 100bar, preferably 35 ~ 55bar.
7. the precipitated silica with particle homogeneity obtained by the described method of one of claim 1-6, BET specific surface area is 100 ~ 250m
2/ g, tap density is 0.20 ~ 0.35cm
3/ g, median D50 is at least 200 μm, 40 order percent of pass>=90.0%, 120 order percent of pass≤12.0%, free-running property≤35 °, moisture≤7.0%.
8. precipitated silica as claimed in claim 7, it is characterized in that, BET specific surface area is 160 ~ 190m
2/ g;
Preferably, tap density is 0.24 ~ 0.28cm
3/ g;
Preferably, median D50 is 200 ~ 300 μm.
9. precipitated silica as claimed in claim 7 or 8, is characterized in that, 40 order percent of pass >=95%;
Preferably, 120 order percent of pass≤10.0%;
Preferably, free-running property≤25 °;
Preferably, moisture is 4.0 ~ 5.0%.
10. the precipitated silica with particle homogeneity as described in one of claim 7-9 is as the purposes of the carrier in feed, agricultural chemicals, medicine and food service industry and anti-caking agent.
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| WO2020140358A1 (en) * | 2019-01-03 | 2020-07-09 | 山东联科科技股份有限公司 | Method for preparing silica microspheres for acidifier carrier |
| CN114349012A (en) * | 2022-01-21 | 2022-04-15 | 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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| WO2020140358A1 (en) * | 2019-01-03 | 2020-07-09 | 山东联科科技股份有限公司 | Method for preparing silica microspheres for acidifier carrier |
| CN114349012A (en) * | 2022-01-21 | 2022-04-15 | 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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| CN104276577B (en) | 2016-08-24 |
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