CN114632469A - Silicon dioxide granulation method and device - Google Patents
Silicon dioxide granulation method and device Download PDFInfo
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- CN114632469A CN114632469A CN202011485675.1A CN202011485675A CN114632469A CN 114632469 A CN114632469 A CN 114632469A CN 202011485675 A CN202011485675 A CN 202011485675A CN 114632469 A CN114632469 A CN 114632469A
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- Prior art keywords
- silicon dioxide
- filter cake
- silica
- granulating
- grinding
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 77
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000005469 granulation Methods 0.000 title claims abstract description 20
- 230000003179 granulation Effects 0.000 title claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000012065 filter cake Substances 0.000 claims description 58
- 239000002245 particle Substances 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 11
- 238000004537 pulping Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 3
- 238000010009 beating Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 2
- 238000011085 pressure filtration Methods 0.000 claims 2
- 239000000843 powder Substances 0.000 abstract description 6
- 239000011325 microbead Substances 0.000 abstract description 4
- 239000000428 dust Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 17
- 239000008187 granular material Substances 0.000 description 12
- 238000005086 pumping Methods 0.000 description 8
- 238000007599 discharging Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004484 Briquette Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a silicon dioxide granulation method and a device, which are used for solving the problems that in the prior art, the powder silicon dioxide product dust pollutes the environment greatly, the powder rate of a briquetting silicon dioxide product is high, the drying cost of microbead silicon dioxide is high, and the like.
Description
Technical Field
The invention relates to the technical field of silicon dioxide production, in particular to a silicon dioxide granulation method and a silicon dioxide granulation device.
Background
The existing granulation method of silica adopts the traditional drying mode, such as a centrifugal atomizer, a pressure spray dryer, and the like.
The product obtained by the centrifugal atomizer is a powdery product, and dust is emitted to pollute the environment in the using process. The powder silica is usually briquetted to obtain briquetted silica products, but the product has high powder rate, uneven briquette particle size distribution, low briquette particle strength and easy particle breakage.
The microbead silicon dioxide product obtained by adopting the pressure spray dryer has uniform particles, but the microbead silicon dioxide product is obtained by directly drying slurry with the solid content of 20-25%, the water content of the slurry is high, the drying temperature is as high as 400-600 ℃, more energy is consumed, and the drying cost is high.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a silicon dioxide granulation method, which aims to solve the problems that powder silicon dioxide products pollute the environment due to large dust, the powder rate of briquetted silicon dioxide products is high, the drying cost of microbead silicon dioxide is high and the like in the prior art.
The second purpose of the invention is to provide the silicon dioxide granulating device which has high degree of maturity and is easy to realize industrial production.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a method of granulating silica comprising the steps of:
(a) carrying out solid-liquid separation on the silicon dioxide slurry to obtain a silicon dioxide filter cake, and cleaning the filter cake;
(b) pulping, grinding and carrying out solid-liquid separation on the filter cake cleaned in the step (a), collecting the filter cake, carrying out dispersion treatment on the filter cake, and granulating to obtain wet silicon dioxide particles;
preferably, a 10-30mm block-shaped filter cake is obtained after the dispersion treatment;
(c) and drying the wet silicon dioxide particles, and screening to obtain the silicon dioxide particles.
Preferably, in the step (a), the solid-liquid separation is filter pressing, and the joint pressure of the filter pressing is 0.6-1.2 MPa.
Preferably, in step (a), the solids content of the filter cake is 20% to 22%.
Preferably, in step (a), the conductivity of the filter cake after the washing is less than or equal to 800 us/cm.
Preferably, in step (b), the beating time is 0.1-0.5 h.
Preferably, in step (b), the milling is ball milling, and the milling medium of the ball milling is zirconium beads with the diameter of 1-5 mm;
more preferably, the ball milling time is 0.1-2 h;
more preferably, the silica particle size in the slurry after said milling is in the range of 2-12 um.
Preferably, in the step (b), the solid-liquid separation is filter pressing, and the pressure of the filter pressing is 6-20MPa, and more preferably 10-15 MPa;
preferably, the solid content of the filter cake after filter pressing is 30-45%.
Preferably, in step (c), the drying temperature is 120-250 ℃, and more preferably 140-200 ℃.
Preferably, in step (c), the silica particles have a particle size in the range of from 1 to 5 mm.
A silicon dioxide granulating device is suitable for the silicon dioxide granulating method and comprises a first plate-and-frame filter press, a cleaning tank, a beater, a grinding device, a second plate-and-frame filter press, a breaker, a granulator, a drying device and a vibrating screen which are connected in sequence;
preferably, the drying device is selected from one or a combination of more of a boiling bed dryer, a belt dryer and a fluidized bed dryer;
preferably, the vibration screen is one or a combination of several of a self-rotating vibration screen, a linear vibration screen, a straight-line vibration screen and an ultrasonic vibration screen.
Compared with the prior art, the invention has the beneficial effects that:
(1) the granulation method of the silicon dioxide provided by the invention is simple and easy to operate, and the obtained granulated silicon dioxide product has high purity and low production cost, and can be used for preparing rubber products, coatings, printing ink, adhesives, silicon rubber products and the like.
(2) The silicon dioxide granulating device provided by the invention has high equipment maturity and is easy to realize industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic connection diagram of a silica granulating apparatus according to an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
A method of granulating silica comprising the steps of:
(a) carrying out solid-liquid separation on the silicon dioxide slurry to obtain a silicon dioxide filter cake, and cleaning the filter cake;
in some preferred embodiments of the present invention, in order to improve the efficiency of solid-liquid separation, a filter cake with a higher solid content is obtained, the solid-liquid separation is filter pressing, and the mold closing pressure of the filter pressing is 0.6-1.2 MPa;
further, the silicon dioxide is precipitated white carbon black, and can be prepared by a sulfuric acid method, a hydrochloric acid method or a carbonic acid method;
further, the solid content of the obtained filter cake is 20% -22%;
further, the conductivity is reduced, the ion content in the white carbon black filter cake can be fully removed, the content of the white carbon black can be effectively improved, the conductivity of the cleaned filter cake is less than or equal to 800us/cm, and the measurement of the conductivity is to dissolve the filter cake in water for testing;
(b) pulping, grinding and carrying out solid-liquid separation on the filter cake cleaned in the step (a), collecting the filter cake, carrying out dispersion treatment on the filter cake, and granulating to obtain wet silicon dioxide particles;
further, a 10-30mm block-shaped filter cake is obtained after dispersion, so that granulation is facilitated;
further, the pulping time is 0.1-0.5 h;
further, after the grinding, the particle size of the silicon dioxide in the slurry is in the range of 2-12 um;
further, in order to achieve a better grinding effect and improve the grinding effect, the grinding is ball milling, and the grinding medium of the ball milling is zirconium beads with the diameter of 1-5 mm; the ball milling time is 0.1-2 h;
further, in order to improve the efficiency of solid-liquid separation and obtain a filter cake with higher solid content, the solid-liquid separation is filter pressing, and the pressure of the filter pressing is 6-20MPa, preferably 10-15 MPa;
further, the solid content of the filter cake after filter pressing is 30-45%;
(c) drying the wet silicon dioxide particles, and screening to obtain silicon dioxide particles;
further, low-temperature drying is adopted, so that energy and cost required by drying are saved, the drying temperature is 120-250 ℃, and the preferable temperature is 140-200 ℃;
further, the particle size of the silica particles ranges from 1 to 5 mm.
A silicon dioxide granulating device is shown in figure 1 and comprises a first plate-and-frame filter press, a cleaning tank, a pulping machine, a grinding device, a second plate-and-frame filter press, a scattering machine, a granulating machine, a drying device and a vibrating screen which are sequentially connected.
Further, the drying device is selected from one or a combination of several of a boiling bed dryer, a belt dryer and a fluidized bed dryer.
Further, the vibration screen is one or a combination of several of a self-rotating vibration screen, a linear vibration screen, a straight-line vibration screen and an ultrasonic vibration screen.
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
The granulation method of silica provided in this embodiment includes the following steps:
(1) pumping the silicon dioxide slurry produced by a precipitation method into a low-pressure plate-and-frame filter press, wherein the mold closing pressure is 0.6MPa, the filter press obtains a filter cake with the solid content of 20%, and the filter cake is cleaned until the conductivity is lower than 800 us/cm;
(2) pulping the cleaned filter cake for 0.1h, and performing ball milling treatment for 0.1h, wherein the grinding medium is zirconium beads with the particle size of 1mm to obtain silicon dioxide slurry with the particle size of 2 um;
(3) pumping the slurry obtained in the step (2) into a high-pressure plate-and-frame filter press, wherein the mold closing pressure is 6MPa, performing high-pressure squeezing to obtain a filter cake with the solid content of 30%, discharging the filter cake, scattering the filter cake to 10mm by a scattering machine, and conveying the filter cake into a granulator for granulation to obtain wet granules with the particle size of 1 mm;
(4) and (3) conveying the wet granules into a dryer, drying for 0.5h at 120 ℃, and screening the dried granules by a vibrating screen to obtain a granulated silicon dioxide product with the particle size of 1mm, wherein the cost is reduced by 700 yuan compared with the traditional pressure spray drying process.
Example 2
The method for granulating silica provided by the embodiment comprises the following steps:
(1) pumping the silicon dioxide slurry produced by a precipitation method into a low-pressure plate-and-frame filter press, wherein the mold closing pressure is 1.2MPa, the filter press obtains a filter cake with the solid content of 22%, and cleaning the filter cake until the conductivity is lower than 800 us/cm;
(2) pulping the cleaned filter cake for 0.5h, and performing ball milling treatment for 2h, wherein the grinding medium is 5mm zirconium beads to obtain silicon dioxide slurry with the particle size of 12 um;
(3) pumping the slurry obtained in the step (2) into a high-pressure plate-and-frame filter press, wherein the mold closing pressure is 20MPa, performing high-pressure squeezing to obtain a filter cake with the solid content of 45%, discharging the filter cake, scattering the filter cake to 30mm by a scattering machine, and conveying the filter cake into a granulator for granulation to obtain wet granules with the size of 5 mm;
(4) and (3) conveying the wet granules into a dryer, drying for 0.1h at 250 ℃, and screening the dried granules by a vibrating screen to obtain a granulated silicon dioxide product with the particle size of 5mm, wherein the cost is reduced by 930 yuan compared with the traditional pressure spray drying process.
Example 3
The granulation method of silica provided in this embodiment includes the following steps:
(1) pumping the silicon dioxide slurry produced by a precipitation method into a low-pressure plate-and-frame filter press, wherein the mold closing pressure is 0.8MPa, the filter press obtains a filter cake with the solid content of 21%, and the filter cake is cleaned until the conductivity is lower than 800 us/cm;
(2) pulping the cleaned filter cake for 0.4h, and performing ball milling treatment for 0.5h, wherein the grinding medium is 2mm zirconium beads to obtain silicon dioxide slurry with the particle size of 4 um;
(3) pumping the slurry obtained in the step (2) into a high-pressure plate-and-frame filter press, wherein the mold closing pressure is 10MPa, performing high-pressure squeezing to obtain a filter cake with the solid content of 35%, discharging the filter cake, scattering the filter cake to 20mm by a scattering machine, and conveying the filter cake into a granulator for granulation to obtain wet granules with the particle size of 3 mm;
(4) and (3) conveying the wet granules into a dryer, drying for 0.4h at 150 ℃, and screening the dried granules by a vibrating screen to obtain a granulated silicon dioxide product with the particle size of 3mm, wherein the cost is reduced by 755 yuan compared with the cost of the traditional pressure spray drying process.
Example 4
The granulation method of silica provided in this embodiment includes the following steps:
(1) pumping the silicon dioxide slurry produced by a precipitation method into a low-pressure plate-and-frame filter press, wherein the mold closing pressure is 1.0MPa, the filter press obtains a filter cake with the solid content of 22%, and the filter cake is cleaned until the conductivity is lower than 800 us/cm;
(2) pulping the cleaned filter cake for 0.3h, and performing ball milling treatment for 1h, wherein the grinding medium is 4mm zirconium beads to obtain silicon dioxide slurry with the particle size of 7 um;
(3) pumping the slurry obtained in the step (2) into a high-pressure plate-and-frame filter press, wherein the mold closing pressure is 15MPa, performing high-pressure squeezing to obtain a filter cake with the solid content of 40%, discharging the filter cake, scattering the filter cake to 10-30mm by a scattering machine, and conveying the filter cake into a granulator for granulation to obtain wet granules with the particle size of 4 mm;
(4) and (3) conveying the wet granules into a dryer, drying for 0.4h at 200 ℃, screening the dried granules by a vibrating screen to obtain a granulated silicon dioxide product with the particle size of 4mm, wherein the cost is reduced by 867 yuan compared with the traditional pressure spray drying process.
Example 5
The silicon dioxide granulating device provided by the embodiment comprises a first plate-and-frame filter press, a cleaning tank, a beater, a grinding device, a second plate-and-frame filter press, a beater, a granulator, a drying device and a vibrating screen which are connected in sequence.
Example 6
The silicon dioxide granulating device provided by the embodiment comprises a first plate-and-frame filter press, a cleaning tank, a beater, a ball mill, a second plate-and-frame filter press, a scattering machine, a granulator, a fluidized bed dryer and a linear vibrating screen which are sequentially connected.
Example 7
The silicon dioxide granulating device provided by the embodiment comprises a first plate-and-frame filter press, a cleaning tank, a pulping machine, a ball mill, a second plate-and-frame filter press, a scattering machine, a granulating machine, a fluidized bed dryer and an ultrasonic vibration sieve which are connected in sequence.
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the above embodiments are merely illustrative of the technical solution of the present invention and are not restrictive; those of ordinary skill in the art will understand that: modifications may be made to the above-described embodiments, or equivalents may be substituted for some or all of the features thereof without departing from the spirit and scope of the present invention; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; it is therefore intended to cover in the appended claims all such alternatives and modifications that are within the scope of the invention.
Claims (10)
1. A method for granulating silica, comprising the steps of:
(a) carrying out solid-liquid separation on the silicon dioxide slurry to obtain a silicon dioxide filter cake, and cleaning the filter cake;
(b) pulping, grinding and carrying out solid-liquid separation on the filter cake cleaned in the step (a), collecting the filter cake, carrying out dispersion treatment on the filter cake, and granulating to obtain wet silicon dioxide particles;
preferably, a 10-30mm block-shaped filter cake is obtained after the dispersion treatment;
(c) and drying the wet silicon dioxide particles, and screening to obtain the silicon dioxide particles.
2. The method for granulating silica as claimed in claim 1, wherein in the step (a), the solid-liquid separation is a press filtration, and the die pressure of the press filtration is 0.6 to 1.2 MPa.
3. A process for granulation of silica according to claim 1, characterized in that in step (a), the solid content of said filter cake is comprised between 20% and 22%.
4. The method for granulating silica according to claim 1, wherein in the step (a), the electric conductivity of the cake after the washing is not more than 800 us/cm.
5. The process for granulation of silica according to claim 1, characterized in that in step (b), the beating time is comprised between 0.1 and 0.5 h.
6. A process for granulation of silica according to claim 1, wherein in step (b), said grinding is ball milling, said ball milling grinding medium being 1-5mm zirconium beads;
preferably, the ball milling time is 0.1-2 h;
preferably, the particle size of the silica in the slurry after said grinding is in the range of 2-12 um.
7. The process for granulation of silica according to claim 1, characterized in that in step (b), said solid-liquid separation is a pressure filtration, the pressure of said pressure filtration being comprised between 6 and 20MPa, preferably between 10 and 15 MPa;
preferably, the solid content of the filter cake after filter pressing is 30-45%.
8. The method for granulating silica as claimed in claim 1, wherein the drying temperature in step (c) is 120-250 ℃, preferably 140-200 ℃.
9. The method for granulating silica as claimed in claim 1, wherein in the step (c), the silica particles have a particle size in the range of 1 to 5 mm.
10. A silica granulating apparatus suitable for use in a silica granulating method as claimed in any one of claims 1 to 9, comprising a first plate and frame filter press, a wash tank, a beater, a grinding apparatus, a second plate and frame filter press, a beater, a granulator, a drying apparatus and a vibrating screen connected in this order;
preferably, the drying device is selected from one or a combination of more of a boiling bed dryer, a belt dryer and a fluidized bed dryer;
preferably, the vibration screen is one or a combination of several of a self-rotating vibration screen, a linear vibration screen, a straight-line vibration screen and an ultrasonic vibration screen.
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| CN202011485675.1A CN114632469A (en) | 2020-12-16 | 2020-12-16 | Silicon dioxide granulation method and device |
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2020
- 2020-12-16 CN CN202011485675.1A patent/CN114632469A/en active Pending
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|---|---|---|---|---|
| US4087254A (en) * | 1974-01-03 | 1978-05-02 | J. M. Huber Corporation | Process for pelletizing wet siliceous particulates |
| CN101734667A (en) * | 2009-12-23 | 2010-06-16 | 昊华宇航化工有限责任公司 | Process for producing precipitated white carbon black by silicon tetrachloride |
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