CN113264531B - Preparation method of granular feed additive silicon dioxide - Google Patents
Preparation method of granular feed additive silicon dioxide Download PDFInfo
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- CN113264531B CN113264531B CN202110710613.4A CN202110710613A CN113264531B CN 113264531 B CN113264531 B CN 113264531B CN 202110710613 A CN202110710613 A CN 202110710613A CN 113264531 B CN113264531 B CN 113264531B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 41
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 34
- 239000003674 animal food additive Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 39
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 39
- 230000032683 aging Effects 0.000 claims abstract description 36
- 238000004537 pulping Methods 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000001694 spray drying Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 64
- 238000006243 chemical reaction Methods 0.000 claims description 45
- 238000001035 drying Methods 0.000 claims description 44
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 18
- 230000005291 magnetic effect Effects 0.000 claims description 16
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000003607 modifier Substances 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 229920003169 water-soluble polymer Polymers 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 229910001385 heavy metal Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000010419 fine particle Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000013461 design Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000003679 aging effect Effects 0.000 description 2
- 239000006224 matting agent Substances 0.000 description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Animal Husbandry (AREA)
- Silicon Compounds (AREA)
Abstract
The preparation method of the granular feed additive silicon dioxide comprises the following steps: a) sodium silicate solution purification treatment, b) first synthesis reaction, c) first cooling and standing treatment, d) first aging treatment, e) second synthesis reaction, f) second cooling and standing treatment, g) second aging treatment, h) third synthesis reaction, i) third cooling and standing treatment, j) third aging treatment, k) filtration washing treatment, l) pulping modification treatment and n) spray drying granulation treatment. The silicon dioxide product prepared by the preparation method has high quality, various properties of the product are obviously improved, the dispersibility and the particle strength of the product in the use process are greatly improved, the anti-caking capacity is strong, the fluidity is strong, and the particle size reaches more than 90% of the 100-mesh screen residue. The compound feed additive is particularly suitable for being applied to the field of feed additives, and can be used as a glidant and an anticaking agent and also can be used as a carrier.
Description
Technical Field
The invention relates to the technical field of silica preparation, in particular to a preparation method of granular feed additive silica.
Background
Silica is an inorganic substance with the chemical formula of SiO 2 The long-range order arrangement of silicon atoms and oxygen atoms forms crystalline silica, and the short-range order or long-range disordered arrangement forms amorphous silica. Silica is a raw material for manufacturing glass, optical fiber, optical instruments, artware, refractory materials and feed additives, and is an important material for scientific research.
The feed additive is a small amount or trace amount of substances added in the feed production, processing and using processes, has little use amount but obvious effect in the feed, has obvious effects in improving animal production performance, guaranteeing animal health, saving feed cost, improving animal product quality and the like, and needs to use silicon dioxide in the additive production process. Taking synthetic silicon dioxide as an example, the existing preparation process generally comprises the steps of taking sodium silicate as a raw material, controlling the concentration of added acid and sodium silicate, synthesizing, washing with water, refining, drying and the like to obtain the product. However, the quality of the silicon dioxide prepared by the existing preparation method is not high, and particularly, the parameter value and the fluidity of the oil absorption value are not ideal enough, so that the application of the product is influenced.
Disclosure of Invention
The invention provides a preparation method of granular feed additive silicon dioxide, which aims to overcome the defects that the quality of the silicon dioxide prepared by the existing preparation method is not high, and obvious effects are difficult to play in the application of the feed additive.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the granular feed additive silicon dioxide comprises the following steps: a) Purifying sodium silicate solution, adding flocculant with the concentration of 0.1-0.2% into sodium silicate solution with the concentration of 0.4-2.0mol/L under the condition of stirring the sodium silicate solution, filtering out impurities separated out from the sodium silicate solution by using a plate frame after stirring for 0.5-2 hours, and obtaining high-purity 0.4-2.0mol/L sodium silicate solution so as to remove impurities and heavy metals in the sodium silicate solution; b) Mixing the sodium silicate solution and water, adding the mixture into a reaction kettle, preparing the solution with the concentration of 0.05-0.5mol/L, quickly heating the sodium silicate solution in the reaction kettle to 60-70 ℃, adding the sulfuric acid solution with the concentration of 10-50% under the condition of stirring the sodium silicate solution until the pH value of the solution after the reaction reaches 5.0-8.0, stopping adding the sulfuric acid solution, and ending the reaction to obtain a first slurry; c) Performing primary aging treatment, namely performing primary aging treatment on the first slurry, wherein the primary aging time is controlled to be 10-30 minutes; e) The second synthesis reaction, the first slurry in the reaction kettle is scattered evenly, and after the temperature is raised to 70 ℃ to 80 ℃, the sodium silicate solution with the concentration of 0.4 mol/L to 2.0mol/L and the sulfuric acid solution with the concentration of 10 percent to 50 percent are added under the condition of stirring the first slurry, a certain amount of modifier is added, the pH value of the reacted solution is controlled to be 8 to 11 by adjusting the flow rates of the two solutions, and the sodium silicate solution and the sulfuric acid solution are stopped to be added after the sodium silicate solution reaches the preset amount, so that the reaction is finished; f) Cooling and standing for the second time, stopping stirring, rapidly cooling the solution in the reaction kettle to 40-50 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel again, thereby obtaining second slurry; g) Performing second aging treatment, namely performing second aging treatment on the second slurry, wherein the second aging time is controlled to be 20-40 minutes; h) A third synthesis reaction, namely uniformly scattering the second slurry in the reaction kettle, quickly heating to 70-90 ℃, ensuring that under the condition of stirring the second slurry, adding a sulfuric acid solution with the concentration of 10-50%, and simultaneously adding a certain amount of modifier until the pH value of the solution after the reaction reaches 3.0-6.0, stopping adding the sulfuric acid solution, and ending the reaction; i) Cooling and standing for the third time, stopping stirring, rapidly cooling the solution in the reaction kettle to 50-60 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel again, thereby obtaining third slurry; j) Performing third aging treatment, namely performing third aging treatment on the third slurry, wherein the third aging time is controlled to be 0.5-2.0 hours; k) Filtering and washing, namely, carrying out press filtration and washing treatment on the third slurry through a press plate frame, so that the content of soluble dissociated salts (such as sulfate) of a filter cake after press filtration and washing treatment is less than 4%, and the solid content of the filter cake is 20% -40%; l) pulping and modifying treatment, namely pulping a filter cake by a pulping machine to prepare fourth slurry, and adding a water-soluble polymer stabilizer with concentration of 0.1-0.2% in the pulping treatment process, wherein the fourth slurry is in a liquid state; n) spray drying granulation treatment, namely drying granulation treatment is carried out on the fourth slurry through spray drying equipment, the fourth slurry is spray dried by a drying tower to prepare granular silicon dioxide, and then the silicon dioxide finished products with different meshes are screened out through the screen mesh of a vibrating screen.
Further, before the first aging treatment in the step c), the first cooling and standing treatment is needed, stirring is stopped, the solution in the reaction kettle is rapidly cooled to 30-40 ℃, and the reaction kettle is kept for a period of time, so that the solution in the reaction kettle becomes gel, and then the first slurry is obtained.
Further, in the pulping treatment in the step k), the water-soluble polymer stabilizer is polyacrylamide, sodium polyacrylate or a combination thereof.
Further, in the step k) of pulping treatment, the pulping treatment is a secondary pulping treatment, and firstly, a filter cake is beaten into coarse pulp with large particle aggregates through a primary beater; then, the coarse pulp is sheared into fine pulp with fine particle aggregates by a secondary beater, and the fine pulp is the fourth pulp.
Further, the silica product in the spray drying treatment in the step l) is required to be subjected to strong magnetic iron removal treatment, and then packaged and bagging is carried out; a strong magnetic rod is arranged on a discharge hole of the packing machine, and magnetic metal impurities in the finished product are effectively removed through the strong magnetic effect of the strong magnetic rod on the finished product.
By adopting the technical scheme, the preparation method has the beneficial effects that the quality of the silicon dioxide is high, the performances of the silicon dioxide are obviously improved, the dispersibility and the particle strength of the silicon dioxide in the use process are greatly improved, the anti-caking capacity is strong, the fluidity is strong, and the particle size reaches more than 90% of the 100-mesh screen residue. The compound feed additive is particularly suitable for being applied to the field of feed additives, and can be used as a glidant and an anticaking agent and also can be used as a carrier. The purity of the silicon dioxide of the product can reach more than 98 percent, and the heavy metal content is low (for example, as is less than 0.5mg/kg, pb is less than 1.0 mg/kg). The DBP absorption value of the silicon dioxide of the product can reach 2.3mL/g-3.5mL/g; the specific surface area is 170-300 square meters per gram.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is a schematic diagram of a spray drying apparatus according to the present invention.
Fig. 3 is a schematic view of a drying drum according to the present invention.
Fig. 4 is a schematic cross-sectional view of a drying drum according to the present invention.
Detailed Description
Specific embodiments of the present invention will be described below with reference to the accompanying drawings.
Reference is made to fig. 1. The preparation method of the granular feed additive silicon dioxide comprises the following steps: a) Purifying sodium silicate solution, adding flocculant with concentration of 0.1-0.2% into sodium silicate solution with concentration of 0.4-2.0mol/L under stirring, filtering out impurities separated out from sodium silicate solution with plate frame after stirring for 0.5-2 hours to obtain high purity 0.4-2.0mol/L sodium silicate solution, and adding flocculant with concentration of 0.1-0.2% for removing impurities and heavy metals in sodium silicate solution. The flocculant can be inorganic salt flocculant such as polyaluminum sulfate, polysilicic acid or aluminum silicate.
b) Mixing the sodium silicate solution and water, adding the mixture into a reaction kettle, preparing the solution with the concentration of 0.05-0.5mol/L, quickly heating the sodium silicate solution in the reaction kettle to 60-70 ℃, adding the sulfuric acid solution with the concentration of 10-50% under the condition of stirring the sodium silicate solution until the pH value of the solution after the reaction reaches 5.0-8.0, and stopping adding the sulfuric acid solution to finish the reaction.
c) Cooling and standing for the first time, stopping stirring, rapidly cooling the solution in the reaction kettle to 30-40 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel, thereby obtaining first slurry; the first cooling and standing treatment is adopted, and the purpose is to keep the solution still to form gel and then to carry out the first aging treatment, so that the solution has no fluidity, and the macromolecules (such as silicon dioxide particles) in the solution are connected with each other to form a space reticular structure, thereby not only improving the effect of the subsequent second aging treatment, but also improving the effect of the modifier in the subsequent second synthesis process, and greatly improving the high oil absorption value performance of the matting agent.
d) And (3) performing primary aging treatment, namely performing primary aging treatment on the primary slurry, wherein the primary aging time is controlled to be 10-30 minutes.
e) And (3) carrying out a second synthesis reaction, namely uniformly scattering the first slurry in the reaction kettle, quickly heating to 70-80 ℃, adding a sodium silicate solution with the concentration of 0.4-2.0mol/L and a sulfuric acid solution with the concentration of 10-50% under the condition of stirring the first slurry, simultaneously adding a certain amount of modifier, controlling the pH value of the reacted solution to be 8-11 by adjusting the flow rates of the sodium silicate solution and the sulfuric acid solution, stopping adding the sodium silicate solution and the sulfuric acid solution when the sodium silicate solution reaches a preset amount, and ending the reaction. The modifier is cetyl trimethyl ammonium bromide or cetyl trimethyl ammonium chloride.
f) Cooling and standing for the second time, stopping stirring, rapidly cooling the solution in the reaction kettle to 40-50 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel again, thereby obtaining second slurry; the second cooling and standing treatment is adopted, and the purpose is to keep the solution still to form gel, and then carry out the second aging treatment and the second synthesis, so that the solution has no fluidity, and the macromolecules (such as silicon dioxide particles) in the solution are connected with each other to form a space reticular structure, thereby not only improving the aging effect of the third time in the subsequent step, but also improving the effect of the modifier in the third synthesis process in the subsequent step, and greatly improving the performance of the matting agent with high oil absorption value.
g) And (3) performing second aging treatment, namely performing second aging treatment on the second slurry, wherein the second aging time is controlled to be 20-40 minutes.
h) And (3) carrying out a third synthesis reaction, namely uniformly scattering the second slurry in the reaction kettle, quickly heating to 70-90 ℃, adding a sulfuric acid solution with the concentration of 10-50% under the condition of stirring the second slurry, adding a certain amount of modifier at the same time, stopping adding the sulfuric acid solution until the pH value of the reacted solution reaches 3.0-6.0, and ending the reaction.
i) Cooling and standing for the third time, stopping stirring, rapidly cooling the solution in the reaction kettle to 50-60 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel again, thereby obtaining third slurry; the third cooling and standing treatment is adopted, and the purpose is to keep the solution stand to form gel and then carry out the second aging treatment, so that the solution has no fluidity, and the macromolecules (such as silicon dioxide particles) in the solution are connected with each other to form a space reticular structure, thereby greatly improving the subsequent third aging effect.
j) And (3) performing third aging treatment, namely performing third aging treatment on the third slurry, wherein the third aging time is controlled to be 0.5-2.0 hours.
k) Filtering and washing, namely, carrying out press filtration and washing treatment on the third slurry through a press plate frame, so that the content of soluble dissociated salts (such as sulfate) of a filter cake after press filtration and washing treatment is less than 4%, and the solid content of the filter cake is 20% -40%;
l) pulping and modifying treatment, namely pulping a filter cake by a pulping machine to obtain fourth slurry, and adding a water-soluble polymer stabilizer with the concentration of 0.1-0.2% (the water-soluble polymer stabilizer is polyacrylamide, sodium polyacrylate or a combination thereof, and the like, so as to increase the viscosity of the slurry and enhance the particle strength of a product) in the pulping treatment process, wherein the fourth slurry is in a liquid state; the pulping treatment is secondary pulping treatment, firstly, a filter cake is subjected to primary pulping operation through a primary pulping machine to prepare coarse pulp, and the rotating speed of the primary pulping machine is controlled to be 60-100 revolutions per minute; then, carrying out secondary pulping operation treatment on the coarse pulp through a secondary pulping machine, and shearing the coarse pulp into fine pulp with fine particle aggregates, wherein the rotating speed of the secondary pulping machine is controlled to be 80-120 r/min; the fine slurry is the fourth slurry.
n) spray drying granulation treatment, namely drying granulation treatment is carried out on the fourth slurry through spray drying equipment, the fourth slurry is spray dried by a drying tower on the fourth slurry to obtain granular silicon dioxide, and then the silicon dioxide with different meshes is screened out through a vibrating screen on the fourth slurry. The silicon dioxide also needs to be subjected to strong magnetic iron removal treatment to obtain a silicon dioxide finished product with strong anti-caking capacity and strong fluidity, and then packaging and bagging are carried out; the method for the strong magnetic iron removal treatment comprises the following steps: a strong magnetic rod is arranged on a discharge hole of the packing machine, and the strong magnetic rod is used for carrying out strong magnetic action on the silicon dioxide, so that magnetic metal impurities in the silicon dioxide are effectively removed.
Reference is made to fig. 2. The spray drying equipment comprises a drying tower 1, a cloth bag collector 2 for collecting silica fine powder and a first vibrating screen 3 for collecting silica particles, wherein a feed inlet of the cloth bag collector 2 is connected with an outlet of one side wall of the drying tower 1, a hot air inlet 10 is formed in the other side wall of the drying tower 1, a powder discharge outlet 20 is formed in the bottom of the cloth bag collector 2, and the first vibrating screen 3 is arranged at an outlet of the bottom of the drying tower 1. The spray drying equipment further comprises a controller 4, a tail gas tower 5, an atomizer 6 for atomizing fourth slurry, a thick slurry tank 7 for storing the fourth slurry, a screw pump 8 for pumping the fourth slurry in the thick slurry tank 7 into the atomizer 6 and entering the drying tower 1, and a draught fan 9 for pumping tail gas generated by the cloth bag collector 2 into the tail gas tower 5, wherein the atomizer 6 is arranged at the top of the drying tower 1, and the screw pump 8, the atomizer 6, the draught fan 9 and the first vibrating screen 3 are controlled by the controller 4. An upper screen 31, a middle screen 32 and a lower screen 33 are arranged in the first vibrating screen 3, and the upper screen 31 is a 60-mesh screen and forms an included angle of-15 degrees with the horizontal; the middle layer screen 32 is an 80-mesh screen and forms an included angle of 15 degrees with the horizontal; the lower screen 33 is a 100 mesh screen and forms an angle of-15 ° with the horizontal. The working process comprises the following steps: after starting, hot air is introduced into the drying tower 1 from the hot air inlet 10, a screw pump, an atomizer, an induced draft fan and a first vibrating screen are respectively opened, fourth slurry in the thick slurry tank is pumped into the atomizer through the screw pump and enters the drying tower 1, fine powder and dry water are pumped into the cloth bag collector 2 through the hot air drying effect, coarser particles enter the first vibrating screen 3 for vibration classification, and particles larger than 60 meshes are collected through the upper screen 31; the 60-80 mesh granules are collected through the middle layer screen 32; particles of 80 mesh to 100 mesh are collected through the lower screen 33, while particles of less than 100 mesh are collected below the first vibrating screen 3. The spray drying equipment has ideal structural design, high automation control degree and fine operation, can separate powder and particles with different granularity, and has convenient production operation and high added value of products.
Reference is made to figures 2, 3 and 4. The spray drying equipment further comprises a drying roller 11 which performs secondary drying treatment on materials in the drying tower 1 and is obliquely arranged, a spiral baffle 110 along the length direction is arranged on the inner side wall of the inner cylinder of the drying roller 11, a first outlet with a first valve 12 and a second outlet with a second valve 13 are arranged at the bottom of the drying tower 1, the first outlet is connected with a feed inlet of the first vibrating screen 3, the second outlet is connected with the feed inlet of the drying roller 11, the drying roller 11 is driven to rotate by a roller motor 15, a second vibrating screen 14 is connected with a discharge outlet of the drying roller 11, the second vibrating screen 14 and the roller motor 15 are also controlled by the controller 4, an upper screen 141 and a lower screen 142 are arranged in the second vibrating screen 14, and the upper screen 141 is a 60-mesh screen and forms an included angle with the horizontal plane by-15 degrees; the lower screen 142 is a 100 mesh screen and is angled at 15 ° to the horizontal. By adopting the design of the drying roller 11, the materials in the drying tower 1 are subjected to secondary drying treatment, the drying degree is high, and a silicon dioxide finished product with high drying strength can be obtained. After the second outlet material of the drying tower 1 enters the inlet at the upper end of the drying roller 11, the controller starts the motor 15, so that the motor 15 drives the drying roller 11 to rotate, the material continuously moves forwards in the drying roller 11, and then enters the second vibrating screen 14 from the outlet below the lower end of the drying roller 11. By adopting the design of the spiral baffle 110, the continuous forward moving path of the material in the drying roller 11 is lengthened, the waiting time of the material in the drying roller 11 is greatly prolonged, and the drying effect of the material is further improved.
The foregoing is merely illustrative of specific embodiments of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modification of the present invention by using the design concept shall fall within the scope of the present invention.
Claims (3)
1. The preparation method of the granular feed additive silicon dioxide is characterized by comprising the following steps: a) Purifying sodium silicate solution, adding flocculant with the concentration of 0.1-0.2% into sodium silicate solution with the concentration of 0.4-2.0mol/L under the condition of stirring the sodium silicate solution, filtering out impurities separated out from the sodium silicate solution by using a plate frame after stirring for 0.5-2 hours, and obtaining high-purity 0.4-2.0mol/L sodium silicate solution so as to remove impurities and heavy metals in the sodium silicate solution; the flocculant is an inorganic salt flocculant of polyaluminium sulfate, polysilicic acid or aluminum silicate; b) Mixing the sodium silicate solution and water, adding the mixture into a reaction kettle, preparing the solution with the concentration of 0.05-0.5mol/L, quickly heating the sodium silicate solution in the reaction kettle to 60-70 ℃, adding the sulfuric acid solution with the concentration of 10-50% under the condition of stirring the sodium silicate solution until the pH value of the solution after the reaction reaches 5.0-8.0, stopping adding the sulfuric acid solution, and ending the reaction to obtain a first slurry; c) Performing primary aging treatment, namely performing primary aging treatment on the first slurry, wherein the primary aging time is controlled to be 10-30 minutes; e) The second synthesis reaction, the first slurry in the reaction kettle is scattered evenly, and after the temperature is raised to 70 ℃ to 80 ℃, the sodium silicate solution with the concentration of 0.4 mol/L to 2.0mol/L and the sulfuric acid solution with the concentration of 10 percent to 50 percent are added under the condition of stirring the first slurry, a certain amount of modifier is added, the pH value of the reacted solution is controlled to be 8 to 11 by adjusting the flow rates of the two solutions, and the sodium silicate solution and the sulfuric acid solution are stopped to be added after the sodium silicate solution reaches the preset amount, so that the reaction is finished; the modifier is cetyl trimethyl ammonium bromide or cetyl trimethyl ammonium chloride; f) Cooling and standing for the second time, stopping stirring, rapidly cooling the solution in the reaction kettle to 40-50 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel again, thereby obtaining second slurry; g) Performing second aging treatment, namely performing second aging treatment on the second slurry, wherein the second aging time is controlled to be 20-40 minutes; h) A third synthesis reaction, namely uniformly scattering the second slurry in the reaction kettle, quickly heating to 70-90 ℃, ensuring that under the condition of stirring the second slurry, adding a sulfuric acid solution with the concentration of 10-50%, and simultaneously adding a certain amount of modifier until the pH value of the solution after the reaction reaches 3.0-6.0, stopping adding the sulfuric acid solution, and ending the reaction; i) Cooling and standing for the third time, stopping stirring, rapidly cooling the solution in the reaction kettle to 50-60 ℃, and standing for a period of time to enable the solution in the reaction kettle to become gel again, thereby obtaining third slurry; j) Performing third aging treatment, namely performing third aging treatment on the third slurry, wherein the third aging time is controlled to be 0.5-2.0 hours; k) Filtering and washing, namely, carrying out press filtration and washing treatment on the third slurry through a press plate frame, so that the content of soluble dissociated salt of a filter cake after press filtration and washing treatment is less than 4%, and the solid content of the filter cake is 20% -40%; l) pulping and modifying treatment, namely pulping a filter cake by a pulping machine to prepare fourth slurry, and adding a water-soluble polymer stabilizer with concentration of 0.1-0.2% in the pulping treatment process, wherein the fourth slurry is in a liquid state; the water-soluble polymer stabilizer is polyacrylamide; n) spray drying granulation treatment, namely drying granulation treatment is carried out on the fourth slurry through spray drying equipment, the fourth slurry is spray dried by a drying tower to prepare granular silicon dioxide, and then silicon dioxide finished products with different meshes are screened out through a screen mesh of a vibrating screen; the silica finished product also needs to be subjected to strong magnetic iron removal treatment to obtain a silica product with high oil absorption value and strong fluidity, and then packaging and bagging are carried out; a strong magnetic rod is arranged on a discharge hole of the packing machine, and magnetic metal impurities in the finished product are effectively removed through the strong magnetic action of the strong magnetic rod on the finished product; the spray drying equipment comprises a drying tower, a cloth bag collector for collecting silica fine powder and a first vibrating screen for collecting silica particles, wherein a feed inlet of the cloth bag collector is connected with an outlet of one side wall of the drying tower, a hot air inlet is formed in the other side wall of the drying tower, a powder discharge hole is formed in the bottom of the cloth bag collector, and the first vibrating screen is arranged at an outlet of the bottom of the drying tower; the spray drying equipment further comprises a controller, a tail gas tower, an atomizer for atomizing fourth slurry, a thick slurry tank for storing the fourth slurry, a screw pump for pumping the fourth slurry in the thick slurry tank to the atomizer and then to enter the drying tower, and an induced draft fan for pumping tail gas generated by the cloth bag collector into the tail gas tower, wherein the atomizer is arranged at the top of the drying tower, and the screw pump, the atomizer, the induced draft fan and the first vibrating screen are controlled by the controller; an upper screen, a middle screen and a lower screen are arranged in the first vibrating screen, and the upper screen is a 60-mesh screen and forms an included angle of-15 degrees with the horizontal; the middle layer screen is an 80-mesh screen and forms an included angle of 15 degrees with the horizontal; the lower layer screen is a 100-mesh screen and forms an included angle of-15 degrees with the horizontal.
2. The method for preparing the granular feed additive silicon dioxide according to claim 1, which is characterized in that: before the first aging treatment in the step c), the first cooling and standing treatment is needed, stirring is stopped, the temperature of the solution in the reaction kettle is quickly reduced to 30-40 ℃, and the solution is kept for a period of time, so that the solution in the reaction kettle becomes gel, and then the first slurry is obtained.
3. The method for preparing the granular feed additive silicon dioxide according to claim 1, which is characterized in that: in the step k) of pulping treatment, the pulping treatment is a secondary pulping treatment, and firstly, a filter cake is beaten into coarse pulp with large particle aggregates through a primary beater; then, the coarse pulp is sheared into fine pulp with fine particle aggregates by a secondary beater, and the fine pulp is the fourth pulp.
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