CN110371986B - Carbon separation reactor, carbon separation method and treatment method of fly ash - Google Patents
Carbon separation reactor, carbon separation method and treatment method of fly ash Download PDFInfo
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- CN110371986B CN110371986B CN201810330278.3A CN201810330278A CN110371986B CN 110371986 B CN110371986 B CN 110371986B CN 201810330278 A CN201810330278 A CN 201810330278A CN 110371986 B CN110371986 B CN 110371986B
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- 239000010881 fly ash Substances 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000000926 separation method Methods 0.000 title abstract description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 184
- 238000003756 stirring Methods 0.000 claims abstract description 128
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 92
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 92
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- 238000007790 scraping Methods 0.000 claims abstract description 34
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 44
- 235000019353 potassium silicate Nutrition 0.000 claims description 31
- 239000007787 solid Substances 0.000 claims description 17
- 239000004115 Sodium Silicate Substances 0.000 claims description 13
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 9
- 238000013461 design Methods 0.000 abstract description 4
- 230000001360 synchronised effect Effects 0.000 abstract description 4
- 238000003763 carbonization Methods 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 67
- 239000000377 silicon dioxide Substances 0.000 description 32
- 235000012239 silicon dioxide Nutrition 0.000 description 22
- 238000000605 extraction Methods 0.000 description 17
- 239000000047 product Substances 0.000 description 17
- 239000003513 alkali Substances 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
Abstract
The invention relates to the field of carbonation, and particularly provides a carbonation reactor, which comprises: carbon dioxide admission line, agitating unit and carbon divide reactor main part, agitating unit includes: the carbon dioxide inlet pipeline is communicated with the carbon dioxide reactor main body and is used for providing a carbon dioxide source; the stirring shaft penetrates through the carbon dioxide gas inlet pipeline and extends into the carbon dioxide reactor main body; the stirring paddle drives stirring through the stirring shaft so that the carbonation reaction in the carbonation reactor is carried out under the stirring condition; and a scraping blade is arranged on the stirring shaft for scraping. The invention provides a carbonization method and a treatment method of fly ash by using the reactor. The carbon separation reactor has the advantages of ingenious design of self-plugging cleaning structure and easy implementation; the stirring and the blockage clearing are synchronous, and the blockage clearing frequency is convenient and adjustable; the blockage is cleared in time, no delay exists, and the blockage clearing effect is good; the carbon content reaction is stable, the inclusion is less, and the product quality is high.
Description
Technical Field
The invention relates to the field of carbonation, in particular to a carbonation reactor, a carbonation method and a fly ash treatment method.
Background
The main components of the fly ash are alumina and silicon dioxide, and account for more than 80-90% of the total weight of the fly ash. The method for extracting the alumina from the fly ash can relieve the shortage of bauxite in China, and is an important way for high-value utilization of the fly ash. In order to improve the economy of extracting aluminum from fly ash and avoid forming new solid waste, it is necessary to research the extraction and utilization technology of silicon dioxide in fly ash and aluminum extraction slag.
CN101993087A proposes that after acid-soluble impurities in fly ash are leached by 20-38% hydrochloric acid at the temperature of 70-95 ℃, alkali is dissolved at the temperature of 130-.
CN101077777B is prepared from sodium silicate solution with high impurity content by two-step carbon separation.
CN102259874A is used for leaching the fly ash or the aluminum extraction residue with alkali liquor at high temperature, the water glass is obtained by solid-liquid separation, and the white carbon black is prepared by adopting a continuous carbon separation method.
The water glass is obtained by alkali dissolution, and the silicon dioxide is extracted by carbon content, which is an important way for utilizing the fly ash and the residue of extracting aluminum. In the whole process, the process for preparing the water glass by alkali dissolution is mature, and the bottleneck exists in extracting the silicon dioxide by the carbon content. In the carbonation reaction process, the pH value of the water glass solution is continuously reduced along with the continuous introduction of carbon dioxide, and the silicon dioxide is very easy to adhere and block the carbonation tube after being precipitated, so that the reaction is difficult to stably carry out or even stop, the product quality is reduced, and the production efficiency is influenced by the stopping and overhauling of the working procedures.
In order to make the carbonation reaction smoothly proceed, as shown in fig. 1, an anti-blocking facility is currently adopted, and when silica is precipitated and adhered and even blocks the carbonation tube, the reaction is ensured to be uninterrupted by on-line dredging. The adoption of the carbon point anti-blocking measure needs frequent manual intervention, has the defects of untimely dredging and after adjustment, is difficult to ensure the stable carbon point reaction, and influences the product quality. For example, the current technology is difficult to prepare the white carbon black with low iron content meeting the requirements of HG/T3061-.
For the reactor anti-blocking, some technical solutions have been proposed in recent years. For example, CN105586488A provides a metallurgical auxiliary material is with preventing blockking up glassware down, prevents that stifled device includes motor, transmission shaft, stirring rake and prevents stifled oar, and the spiral prevents stifled oar and gos deep into the discharge gate deeply, can effectively prevent metallurgical auxiliary material jam, extrusion blocking, formation cavity etc. in the glassware down, ensures that metallurgical auxiliary material unloading lasts evenly, eliminates the untimely inhomogeneous bad influence to balling quality and efficiency of unloading.
CN205073961U provides an anti-clogging crystallization kettle stirring paddle, including cauldron top locating rack, anchor type stirring paddle and agitator motor. The anchor type stirring paddle is provided with a conical crushing head and an electric heating body, and crystals at the bottom of the kettle can be crushed and removed through two modes of crushing and heating dissolution, so that blockage is prevented.
CN205868260U provides a stirred tank of antiseized knot putty, including reation kettle body, anchor stirring rake, doctor-bar and prevent stifled paddle etc.. The scraping blade is arranged on the side surface and the bottom of the anchor type stirring paddle through bolts, so that materials are prevented from being bonded on the kettle body. The fixed plate is connected with the bottom of the stirring shaft in a welding mode, the anti-blocking paddle is connected with the fixed plate through a bolt, and materials are prevented from settling on the bottom valve short pipe to form blocking.
Therefore, the technical scheme mainly aims at solving the problem that the solid material discharging outlet of the discharging device is blocked or the crystal and the precipitate at the bottom of the reactor block the outlet, and cannot be applied to the blockage prevention and blockage removal of the carbon branched pipe.
Disclosure of Invention
The invention aims to provide a reactor and a carbonation method which can continuously carry out carbonation reaction and can automatically clear blockage of a carbon dioxide inlet pipeline and a treatment method of fly ash.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a carbonation reactor comprising: carbon dioxide admission line, agitating unit and carbon divide reactor main part, agitating unit includes: a stirring shaft and a stirring paddle, wherein,
the carbon dioxide inlet pipeline is communicated with the carbonation reactor main body and is used for providing a carbon dioxide source;
the stirring shaft penetrates through the carbon dioxide gas inlet pipeline and extends into the carbon dioxide reactor main body;
the stirring paddle drives stirring through the stirring shaft so that the carbonation reaction in the carbonation reactor is carried out under the stirring condition;
and a scraper is arranged on the stirring shaft and used for scraping cemented adhesion solids generated in the discharge section of the carbon dioxide gas inlet pipeline in the carbon dioxide reaction process.
According to a second aspect of the present invention there is provided a carbonation process carried out in a carbonation reactor according to the present invention, the process comprising: conveying a carbon dioxide source to the inside of a carbonation reactor main body through the carbon dioxide gas inlet pipeline to contact with a sodium silicate source to carry out carbonation reaction, starting the stirring device to enable the carbonation reaction to be carried out under a stirring condition, simultaneously driving a scraping blade on a stirring shaft to work along with the stirring shaft, and scraping and removing cemented adhesion solids generated at a discharge section of the carbon dioxide gas inlet pipeline by the scraping blade in the carbonation reaction process.
According to a third aspect of the present invention, there is provided a method of treating fly ash, the method comprising: (1) extracting water glass from the fly ash;
(2) and taking the water glass as the sodium silicate source to carry out the carbonation reaction according to the method of the invention.
The carbon separation reactor has the following main advantages in the specific application process:
1. the reactor self-cleaning structure is ingenious in design and easy to implement;
2. the stirring and the blockage clearing are synchronous, and the blockage clearing frequency is convenient and adjustable;
3. the blockage is cleared in time, no delay exists, and the blockage clearing effect is good;
4. the carbon content reaction is stable, the inclusion is less, and the product quality is high.
The traditional carbonation reaction vessel is adopted, the water glass extracted by the extraction process of the fly ash, particularly the water glass obtained by alkali dissolution of the high-alumina fly ash and the aluminum extraction residue thereof, has complex composition and high impurity content, a carbon dioxide gas inlet pipeline is easy to block in the carbonation process, so that the flow is unstable or even interrupted, the reaction is influenced to be stably carried out, a large amount of impurities enter the silicon dioxide, the product quality is reduced, and the high-end application is difficult to carry out. The high-quality silicon dioxide raw material can be successfully extracted and obtained when the carbonation reactor is applied to the carbonation reaction of the water glass extracted by the extraction process of the fly ash, particularly the high-alumina fly ash and the aluminum extraction residue thereof through the alkali dissolution, and specifically, the carbonation reactor has the advantages that the stirring shaft is arranged in the carbon dioxide gas inlet pipeline, the scraping blade is arranged on the stirring shaft and is tightly matched with the inner surface of the carbon dioxide gas inlet pipeline, the scraping blade is driven by the stirring shaft, the scraping blade synchronously cleans the carbon dioxide gas inlet pipeline while the stirring blade disperses the full contact reaction of the carbon dioxide and the water glass, the adhered silicon dioxide cemented solid is removed, the deposition and the blockage are prevented, and the stable proceeding of the carbonation reaction is ensured.
In summary, the present invention has at least the following technical effects:
(1) aiming at the characteristics and technical bottleneck of the carbonation reaction, the existing carbonation stirring reactor is redesigned, and a self-blockage removal structure is introduced, so that the implementation is easy and the effect is obvious;
(2) the coaxial design is adopted, the stirring and the blockage clearing are synchronous, the self-blockage clearing is realized, the frequency is convenient and adjustable, and the adaptability is strong;
(3) the self-cleaning adopts an active mode, so that early-adhered silica cemented solids can be cleaned, the pipeline is effectively prevented from being blocked by sediment accumulation, and the cleaning is timely and has good effect;
(4) based on the characteristics of the reactor, the self-cleaning and blocking carbonation reactor realizes the stable carbonation process, greatly improves the product quality and can greatly reduce the Fe content in carbonation products.
Drawings
FIG. 1 is a prior art carboneous reactor;
FIG. 2 is a carbonator reactor according to one embodiment of the present invention.
Description of the reference numerals
1 reactor body 2 stirring shaft
3 stirring paddle 4 carbon dioxide gas inlet pipeline
5 anti-blocking valve 6 scraping blade
7 stirring motor
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, the use of directional terms such as "upper, lower, left, right" generally means upper, lower, left, right, and the like with reference to the accompanying drawings, unless otherwise specified; "inner and outer" refer to the inner and outer contours of the component or assembly itself.
The carbonation reactor of the invention comprises: carbon dioxide admission line, agitating unit and carbon divide reactor main part, agitating unit includes: the carbon dioxide inlet pipeline is communicated with the carbon dioxide reactor main body and is used for providing a carbon dioxide source; the stirring shaft penetrates through the carbon dioxide gas inlet pipeline and extends into the carbon dioxide reactor main body; the stirring paddle drives stirring through the stirring shaft so that the carbonation reaction in the carbonation reactor is carried out under the stirring condition; and a scraper is arranged on the stirring shaft and used for scraping cemented adhesion solids generated in the discharge section of the carbon dioxide gas inlet pipeline in the carbon dioxide reaction process.
In the invention, the cementing and adhering solid generated in the discharging section is a concept well known to those skilled in the art, and specific examples are silica generated in the carbon component and water glass and alkali liquor wrapped by the silica, and the cementing and adhering solid is formed at the discharging opening of the carbon component tube under the action of dry air flow, and in severe cases, the air flow is blocked and the carbon component tube is blocked. The invention is not described in detail here.
According to a preferred embodiment of the present invention, there is preferably a gap between the wiper and the carbon dioxide inlet duct, more preferably the gap is less than 1 mm. The gap is preferably in the range of the gap, so that the scraper can be conveniently used for clearing and fully clearing the blockage, and the quality of a final carbon content product can be ensured.
According to a preferred embodiment of the present invention, the scraping blades are preferably evenly spaced along the circumferential direction of the stirring shaft. According to the arrangement, the scraping blade can be cleaned sufficiently, and the quality of a final carbon content product can be ensured.
According to a preferred embodiment of the present invention, the projected area of the blades arranged at the same axial height of the stirring shaft on a horizontal plane perpendicular to the stirring shaft is less than 50%, preferably 10-20%, of the cross-sectional area of the carbon dioxide inlet duct at the same axial height. By adopting the arrangement, the quality of the product obtained by the reactor used for the carbonation reaction can be greatly improved.
According to a preferred embodiment of the present invention, a plurality of scraper layers are arranged in parallel along the axial direction of the stirring shaft. By adopting the arrangement, the scraper can be cleaned sufficiently, and the quality of products obtained by the reactor for the carbonation reaction can be greatly improved.
According to a preferred embodiment of the invention, two adjacent scraper layers are staggered. By adopting the arrangement, the scraper can be cleaned sufficiently, and the quality of products obtained by the reactor for the carbonation reaction can be greatly improved.
According to a preferred embodiment of the present invention, the discharging section is a distance section from the discharging port of the carbon dioxide inlet pipe to 10% -30% of the total length of the carbon dioxide inlet pipe.
According to the method of the present invention, the stirring device may be manual or automatic, and when the stirring device is automatic, preferably, the stirring device further comprises a stirring motor for driving the stirring shaft to rotate.
The choice of the stirring motor can be a matter of routine choice and arrangement in the field, for which the invention is not particularly limited and will not be described in detail here.
The stirring paddle is only required to drive stirring through the stirring shaft so that the carbonation reaction in the carbonation reactor can be carried out under the stirring condition, the arrangement mode of the stirring paddle is not particularly required, the stirring paddle can be arranged according to the conventional arrangement mode in the field, and the form and the material selection of the stirring paddle can refer to the conventional arrangement mode in the field and the conventional materials in the field, which are not described in detail herein.
According to one embodiment of the invention, the stirring paddle is arranged at the bottom end of a stirring shaft communicated with the carbon dioxide reactor main body, wherein a scraping blade is arranged at the bottom end of the stirring shaft and is used for scraping the cementing and adhering solids of the carbon dioxide gas inlet pipeline.
According to an embodiment of the present invention, the stirring device includes: stirring motor, (mixing) shaft and stirring rake, wherein, preferentially the (mixing) shaft pass the carbon dioxide admission line with carbon divides reactor main part intercommunication, stirring motor is used for driving the (mixing) shaft rotates.
According to the scheme of the invention, the stirring paddle and the blockage removing scraping blade share the stirring shaft. During specific use, the minimum stirring speed can be set according to the mixing and stirring effect of the carbon slurry, for example, 30-150 rpm. Meanwhile, the blockage can be cleared by adopting a large stirring rotating speed according to the blockage of the carbon dioxide gas inlet pipeline and the equipment condition. That is, the reactor of the present invention, effectively removes clogging by increasing the rotation speed, for example, 300rpm, at a low stirring rotation speed of the silica-cemented solid adhered to the carbon dioxide gas inlet pipe by the carbon content reaction.
The self-plugging cleaning principle of the reactor disclosed by the invention is as follows: and (3) placing all or part of the stirring shaft in the carbon dioxide gas inlet pipeline, and arranging a blockage cleaning scraper on the stirring shaft close to the outlet of the carbon dioxide gas inlet pipeline. Through the (mixing) shaft drive for when stirring rake dispersion carbon dioxide and water glass fully contact reaction, the epaxial doctor-bar of (mixing) is in step cleared up carbon dioxide inlet line and is blocked up, gets rid of the glued solid of silica of adhesion, prevents deposit and jam, ensures the steady of going on of carbon dioxide reaction.
The self-blockage-removing carbonation reactor provided by the invention can adopt an active and frequency-modulation self-blockage-removing mode, effectively solves the problem that silicon dioxide blocks a carbon dioxide gas inlet pipeline during water glass carbon time sharing, reduces the impurity content and improves the purity of the silicon dioxide.
According to the scheme of the invention, the stirring paddle can be provided with a plurality of layers of stirring blades, preferably 1-3 layers of axial flow paddles, forms downward jet flow along the axial direction, effectively washes the bottom of the reactor main body and prevents solid particles from settling and gathering.
According to the arrangement scheme of the reactor, the self-plugging-cleaning carbonation reactor is suitable for all application scenes of preparing silicon dioxide from water glass carbonation, and is particularly suitable for the carbonation scenes of water glass obtained by alkali dissolution of fly ash and aluminum extraction residues thereof.
The carbonation method is carried out in the carbonation reactor, and specifically comprises the following steps: conveying a carbon dioxide source to the inside of a carbonation reactor main body through the carbon dioxide gas inlet pipeline to contact with a sodium silicate source to carry out carbonation reaction, starting the stirring device to enable the carbonation reaction to be carried out under a stirring condition, simultaneously driving a scraping blade on a stirring shaft to work along with the stirring shaft, and scraping and removing cemented adhesion solids generated at a discharge section of the carbon dioxide gas inlet pipeline by the scraping blade in the carbonation reaction process. The quality of the product obtained by the carbonation method is greatly improved.
The invention has no special requirements on the specific formula and composition of the carbon dioxide source, and the carbon dioxide source is selected according to the conventional method, and according to a preferred embodiment of the invention, the carbon dioxide source and the carbon dioxide source are mixed and stirredOxidation of CO in carbon sources2The concentration of the gas is 30 vol% or more.
The invention has no special requirements on the specific formula and the composition of the sodium silicate source, and the sodium silicate is selected according to the conventional method, and according to a preferred embodiment of the invention, the concentration of the sodium silicate in the sodium silicate source is 8-15 wt%.
The invention has no special requirements on the condition of the carbonation reaction, and the carbonation reaction can be selected according to the conventional method, and according to a preferred embodiment of the invention, the condition of the carbonation reaction comprises the following steps: the pH value is 7-12.
The carbonation reactor is particularly suitable for being applied to the carbonation reaction of water glass extracted by the extraction process of fly ash, particularly high-alumina fly ash and aluminum extraction residues thereof through alkali dissolution, and can successfully extract and obtain high-quality silicon dioxide raw materials.
According to a preferred embodiment of the present invention, the method for treating fly ash of the present invention comprises: (1) extracting water glass from the fly ash; (2) and taking the water glass as the sodium silicate source to carry out the carbonation reaction according to the method of the invention.
According to the invention, for the preparation of the water glass, reference can be made to the process conditions used in the technologies of CN101993087A, CN101077777B, CN102259874A and the like. The invention is not particularly limited and will not be described in detail herein.
The traditional carbonation reaction vessel is adopted, the water glass extracted by the extraction process of the fly ash, particularly the water glass obtained by alkali dissolution of the high-alumina fly ash and the aluminum extraction residue thereof, has complex composition and high impurity content, a carbon dioxide gas inlet pipeline is easy to block in the carbonation process, so that the flow is unstable or even interrupted, the reaction is influenced to be stably carried out, a large amount of impurities enter the silicon dioxide, the product quality is reduced, and the high-end application is difficult to carry out. The high-quality silicon dioxide raw material can be successfully extracted and obtained when the carbonation reactor is applied to the carbonation reaction of the water glass extracted by the extraction process of the fly ash, particularly the high-alumina fly ash and the aluminum extraction residue thereof through the alkali dissolution, and specifically, the carbonation reactor has the advantages that the stirring shaft is arranged in the carbon dioxide gas inlet pipeline, the scraping blade is arranged on the stirring shaft and is tightly matched with the inner surface of the carbon dioxide gas inlet pipeline, the scraping blade is driven by the stirring shaft, the scraping blade synchronously cleans the carbon dioxide gas inlet pipeline while the stirring blade disperses the full contact reaction of the carbon dioxide and the water glass, the adhered silicon dioxide cemented solid is removed, the deposition and the blockage are prevented, and the stable proceeding of the carbonation reaction is ensured.
In summary, the present invention has at least the following technical effects:
(1) aiming at the characteristics and technical bottleneck of the carbonation reaction, the existing carbonation stirring reactor is redesigned, and a self-blockage removal structure is introduced, so that the implementation is easy and the effect is obvious;
(2) the coaxial design is adopted, the stirring and the blockage clearing are synchronous, the self-blockage clearing is realized, the frequency is convenient and adjustable, and the adaptability is strong;
(3) the self-cleaning adopts an active mode, so that early-adhered silica cemented solids can be cleaned, the pipeline is effectively prevented from being blocked by sediment accumulation, and the cleaning is timely and has good effect;
(4) based on the characteristics of the reactor, the self-cleaning and blocking carbonation reactor realizes the stable carbonation process, greatly improves the product quality and can greatly reduce the Fe content in carbonation products.
The carbonation reactor and the carbonation process and the use thereof according to the present invention will now be described by way of the following examples.
The specific arrangement of the carbonation reactor adopted in the following embodiment of the invention is shown in fig. 2, and specifically comprises:
the carbonation reactor comprises: carbon dioxide inlet line 4, agitating unit and carbonization reactor main part 1, agitating unit includes: a stirring shaft 2, a stirring paddle 3 and a stirring motor 7, wherein,
the carbon dioxide inlet pipeline 4 is communicated with the carbonation reactor main body 1 and is used for providing a carbon dioxide source;
the stirring shaft 2 penetrates through the carbon dioxide gas inlet pipeline 4 and extends into the carbon dioxide reactor main body 1;
the stirring paddle 3 drives stirring through the stirring shaft 2 to enable the carbonation reaction in the carbonation reactor main body 1 to be carried out under the stirring condition;
a scraping blade 6 is arranged on the stirring shaft and used for scraping cemented adhesion solids generated in the discharge section of the carbon dioxide gas inlet pipeline in the carbon dioxide reaction process; a gap is formed between the scraping piece and the carbon dioxide gas inlet pipeline, and the distance of the gap is 0.5 mm;
the scraping pieces 6 are uniformly arranged at intervals along the circumferential direction of the stirring shaft 2;
2 scraper layers which are parallel and staggered are arranged along the axial direction of the stirring shaft;
the projection area of the scraping blades arranged on the same axial height of the stirring shaft on a horizontal plane vertical to the stirring shaft is 15% of the cross-sectional area of the carbon dioxide inlet pipeline on the same axial height;
the discharge section is a distance section from a discharge hole of the carbon dioxide gas inlet pipeline to 20% of the total length of the carbon dioxide gas inlet pipeline.
The specific arrangement of the carbonation reactor adopted by the following comparative examples is shown in figure 1, and specifically comprises the following steps:
the carbonation reactor comprises: carbon dioxide inlet line 4, agitating unit and carbonization reactor main part 1, agitating unit includes: a stirring shaft 2, a stirring paddle 3 and a stirring motor 7, wherein,
the carbon dioxide inlet pipeline 4 is communicated with the carbonation reactor main body 1 and is used for providing a carbon dioxide source;
the stirring shaft 2 extends into the carbon content reactor main body 1;
the stirring paddle 3 drives stirring through the stirring shaft 2 to enable the carbonation reaction in the carbonation reactor main body 1 to be carried out under the stirring condition;
an anti-blocking valve 5 is arranged on the carbon dioxide inlet pipeline and used for clearing the carbon dioxide inlet pipeline;
the blockage removing process is to ensure that the reaction is not interrupted by on-line dredging when the silicon dioxide is separated out and adhered and even blocks a carbon dioxide inlet pipeline.
Preparation of example 1
The chemical components of the high-alumina fly ash are shown in the table 1.
TABLE 1 analysis of chemical composition (in weight percent) of high alumina fly ash
| SiO2 | Al2O3 | TFe2O3 | CaO | TiO2 | C |
| 27.69 | 48.90 | 2.20 | 3.97 | 1.69 | 6 |
Weighing sodium hydroxide according to the molar ratio of the sodium hydroxide to the silicon dioxide of 2.0, and preparing an alkali solution with the mass concentration of 10%. Mixing with the fly ash in the table 1, stirring and reacting for 60min at 95 ℃, and filtering to obtain the water glass.
Preparation of example 2
The chemical components of the residue after the acid extraction of the high-alumina fly ash are shown in the table 2.
TABLE 2 chemical composition analysis (in weight%) of residue from acid extraction of aluminum
| SiO2 | Al2O3 | TFe2O3 | CaO | TiO2 | C |
| 60.04 | 13.24 | 1.64 | 1.35 | 3.24 | 17 |
Sodium hydroxide was measured out in such a manner that the molar ratio of sodium hydroxide to silicon dioxide was 1.3, and an alkali solution having a mass concentration of 30% was prepared. Mixing with the fly ash shown in the table 2, stirring and reacting for 60min at 135 ℃, cooling and filtering to obtain the water glass.
Example 1
The water glass obtained in preparation example 1 was taken, the self-cleaning carbon-separation reactor provided by the invention in fig. 2 was used, carbon separation was carried out at 80 ℃, the reaction was stable, the end-point pH value was 8.5, precipitated silica was obtained by filtration, and the iron oxide content after washing and drying was 83 ppm.
Example 2
The water glass obtained in preparation example 2 was taken, the self-cleaning carbon-separation reactor provided by the invention in fig. 2 was used, carbon separation was carried out at 80 ℃, the reaction was stable, the end-point pH value was 8.5, precipitated silica was obtained by filtration, and the iron oxide content after washing and drying was 135 ppm.
Comparative example 1
Taking the water glass obtained in the preparation example 1, adopting a traditional carbonation reaction vessel shown in figure 1, carrying out carbonation reaction at 80 ℃, leading the airflow to be unstable and to generate 8 times of blockage, leading the pH value at the end point to be 8.5, filtering to obtain precipitated silicon dioxide, and leading the content of iron oxide after washing and drying to be 570 ppm.
Comparative example 2
Taking the water glass obtained in the preparation example 2, adopting a traditional carbonation reaction vessel shown in figure 1, carrying out carbonation reaction at 80 ℃, leading the airflow to be unstable and to be blocked for 9 times, leading the pH value at the end point to be 8.5, filtering to obtain precipitated silicon dioxide, and leading the content of iron oxide after washing and drying to be 850 pm.
As can be seen from the example 1 and the comparative example 1, after the high-alumina fly ash is subjected to alkali dissolution and desilication, the self-cleaning carbon separation reactor provided by the invention is adopted for carbon separation, the reaction is stable, and the iron content in the product is reduced from 570ppm to 83 ppm.
As can be seen from the example 2 and the comparative example 2, after the alkaline dissolution desilication is carried out on the aluminum extraction residue by the acid method, the self-cleaning carbonation reactor provided by the patent is adopted for carbonation, the reaction is stable, and the iron content in the product is reduced from 850ppm to 135 ppm.
It can be seen from the examples and comparative examples that the self-cleaning carbon separation reactor provided by the invention can ensure the stable carbon separation process, improve the purity of extracted silicon dioxide, and meet the requirements of white carbon black and high-quality silicon dioxide raw materials.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A carbonation reactor, the reactor comprising: carbon dioxide admission line, agitating unit and carbon divide reactor main part, agitating unit includes: a stirring shaft and a stirring paddle, wherein,
the carbon dioxide inlet pipeline is communicated with the carbonation reactor main body and is used for providing a carbon dioxide source;
the stirring shaft penetrates through the carbon dioxide gas inlet pipeline and extends into the carbon dioxide reactor main body;
the stirring paddle drives stirring through the stirring shaft so that the carbonation reaction in the carbonation reactor is carried out under the stirring condition;
a scraping blade is arranged on the stirring shaft and used for scraping cemented adhesion solids generated in the discharge section of the carbon dioxide gas inlet pipeline in the carbon dioxide reaction process; the projection area of the scraping blades arranged on the same axial height of the stirring shaft on a horizontal plane vertical to the stirring shaft is less than 50% of the cross sectional area of the carbon dioxide inlet pipeline on the same axial height.
2. The reactor according to claim 1, wherein the wiper has a gap with the carbon dioxide inlet duct, the gap being less than 1mm apart.
3. The reactor according to claim 1, wherein the blades are uniformly spaced along a circumferential direction of the stirring shaft.
4. The reactor according to claim 1, wherein the projected area of the blades arranged on the same axial height of the stirring shaft on a horizontal plane perpendicular to the stirring shaft is less than 10-20% of the cross-sectional area of the carbon dioxide inlet pipe on the same axial height.
5. The reactor according to any one of claims 1 to 4, wherein a plurality of scraper layers are arranged in parallel along the axial direction of the stirring shaft.
6. The reactor of claim 5, wherein adjacent two scraper layers are staggered.
7. The reactor according to any one of claims 1 to 4, wherein the discharge section is a distance section from a discharge port of the carbon dioxide inlet pipe to 10 to 30% of the total length of the carbon dioxide inlet pipe.
8. A carbonation process, characterised in that it is carried out in a carbonation reactor according to any one of the claims from 1 to 7, the process comprising: conveying a carbon dioxide source to the inside of a carbonation reactor main body through the carbon dioxide gas inlet pipeline to contact with a sodium silicate source to carry out carbonation reaction, starting the stirring device to enable the carbonation reaction to be carried out under a stirring condition, simultaneously driving a scraping blade on a stirring shaft to work along with the stirring shaft, and scraping and removing cemented adhesion solids generated at a discharge section of the carbon dioxide gas inlet pipeline by the scraping blade in the carbonation reaction process.
9. The method of claim 8, wherein,
CO in the carbon dioxide source2The concentration of the gas is above 30 volume percent;
the concentration of sodium silicate in the sodium silicate source is 8-15 wt%;
the conditions of the carbonation reaction comprise: the pH value is 7-12.
10. A method of treating fly ash, the method comprising:
(1) extracting water glass from the fly ash;
(2) the carbonation reaction is carried out by the method according to claim 8 or 9 using the water glass as the sodium silicate source.
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