CN111410199A - White carbon black production device and preparation method - Google Patents
White carbon black production device and preparation method Download PDFInfo
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- CN111410199A CN111410199A CN202010378977.2A CN202010378977A CN111410199A CN 111410199 A CN111410199 A CN 111410199A CN 202010378977 A CN202010378977 A CN 202010378977A CN 111410199 A CN111410199 A CN 111410199A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000006229 carbon black Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- 239000006185 dispersion Substances 0.000 claims abstract description 55
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 43
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 43
- 239000012528 membrane Substances 0.000 claims abstract description 40
- 230000005540 biological transmission Effects 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 30
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 239000004115 Sodium Silicate Substances 0.000 claims description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000012043 crude product Substances 0.000 claims description 10
- 235000019353 potassium silicate Nutrition 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 9
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000004537 pulping Methods 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000012066 reaction slurry Substances 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 15
- 239000007789 gas Substances 0.000 description 71
- 239000007788 liquid Substances 0.000 description 13
- 229960001866 silicon dioxide Drugs 0.000 description 12
- 235000012239 silicon dioxide Nutrition 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000010586 diagram Methods 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000010058 rubber compounding Methods 0.000 description 4
- 229960004029 silicic acid Drugs 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000005273 aeration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
-
- 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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
-
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention provides a production device and a preparation method of white carbon black, which comprises the following steps: the device comprises a power device, a reaction kettle, a hollow shaft, dispersing blades and a dispersing membrane; the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing membrane are all arranged inside the reaction kettle; a driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate; the dispersing blades are hollow inside, and the hollow shaft is connected with the dispersing blades; the dispersing blades are provided with air outlet holes communicated with the hollow part inside, the surfaces of the dispersing blades are connected with dispersing membranes, and one sides of the dispersing membranes, which are tightly attached to the dispersing blades, are communicated with the air outlet holes; the hollow shaft is provided with a shaft gas transmission port so as to transmit gas to the hollow shaft, the dispersing blades and the dispersing membrane in sequence through the gas transmission port. Carbon dioxide gas required by producing the white carbon black is dispersed by the dispersion film and then enters the reaction liquid, a special high-pressure pump is not required for conveying, and the dispersed carbon dioxide can be uniformly dispersed in the reaction liquid by utilizing the rotation of the dispersion blade, so that the production of the white carbon black is facilitated.
Description
Technical Field
The invention relates to the technical field of white carbon black production, and particularly relates to a production device and a preparation method of white carbon black.
Background
White carbon black is a general term for white powdery X-ray amorphous silicic acid and silicate products, mainly referring to precipitated silica, fumed silica and ultrafine silica gel, and also including powdery synthetic aluminum silicate, calcium silicate, and the like. The white carbon black is a porous substance, the composition of the white carbon black can be represented by SiO2 & nH2O, wherein nH2O exists in the form of surface hydroxyl, the white carbon black can be dissolved in caustic alkali and hydrofluoric acid, is not dissolved in water, solvent and acid (except the hydrofluoric acid), and has high temperature resistance, non-combustibility, no odor and good electrical insulation.
However, the production process of the white carbon black at present involves carbon dioxide, and the carbon dioxide needs to be uniformly mixed in the reaction solution, but the existing dispersion method mainly depends on a stirring mode, and cannot achieve a good uniform mixing effect.
Therefore, a better white carbon black production scheme is needed at present.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a production device and a preparation method of white carbon black, carbon dioxide gas required for producing the white carbon black is dispersed by a dispersion film and then enters into reaction liquid, a special high-pressure pump is not required for conveying, and the dispersed carbon dioxide can be uniformly dispersed in the reaction liquid by utilizing the rotation of a dispersion blade, so that the production of the white carbon black is facilitated.
Specifically, the present invention proposes the following specific examples:
the embodiment of the invention provides a white carbon black production device, which comprises: the device comprises a power device, a reaction kettle, a hollow shaft, dispersing blades and a dispersing membrane;
the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing membrane are all arranged inside the reaction kettle;
the driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate;
the dispersing blades are hollow, the hollow shaft is connected with the dispersing blades, and the hollow part of the hollow shaft is communicated with the hollow parts of the dispersing blades;
the dispersing blades are provided with air outlet holes communicated with the hollow part inside, the surfaces of the dispersing blades are connected with the dispersing membrane, and one side of the dispersing membrane close to the dispersing blades is communicated with the air outlet holes;
the hollow shaft is provided with a shaft gas transmission port, so that gas is transmitted to the hollow shaft, the dispersing blades and the dispersing membrane in sequence through the gas transmission port.
In a specific embodiment, the method further comprises the following steps: a dispersion plate; a plate input port is formed in the dispersion plate;
the dispersion plate is hollow, and the first surface of the dispersion plate is also provided with an air outlet communicated with the hollow part;
the first surface of the dispersion plate is provided with the dispersion film; the other side of the dispersion plate is fixed on the inner wall of the reaction kettle.
In a specific embodiment, the dispersion film is a multilayer metal sintered mesh.
In a particular embodiment, the filtration precision of the dispersion membrane is between 1 and 50 μm.
In a specific embodiment, the dispersion membrane is connected to the liquid-facing surface of the dispersion blade.
In a specific embodiment, the method further comprises the following steps: a sealing box; the sealing box is sleeved on the shaft gas transmission port to ensure the sealing performance when gas is transmitted to the hollow shaft.
In a specific embodiment, the method further comprises the following steps: a heater; the heater is arranged on the reaction kettle and used for heating the reaction kettle.
In a particular embodiment, the heater comprises: heating wires, or steam coils, or jacketed steam heaters.
The embodiment of the invention also provides a method for preparing white carbon black based on the white carbon black production device, which is applied to the following steps:
injecting the water glass diluent into the reaction kettle, and starting a power device to stir and heat the stirring paddle;
inputting carbon dioxide into the water glass diluent, controlling the reaction temperature range to be 50-90 ℃, and stopping ventilation after the ventilation time is 5-45 min;
continuously introducing carbon dioxide gas into the reaction solution, controlling the reaction temperature to be 70-95 ℃, and stopping introducing the gas after the introducing time is 10-45 min;
keeping the reaction temperature within the range of 70-95 ℃, starting the power device to stir for 10-150min, and stopping the reaction when the pH value of the reaction solution is controlled to be 5.5-10.0;
and filtering and washing the reaction slurry to obtain a crude product, and pulping and spray-drying the crude product to obtain a nano-silicon dioxide product.
In a specific embodiment, the water glass diluent is prepared by using a commercial grade sodium silicate solution with a Baume degree of 38 and a modulus of 3-4.
Therefore, the embodiment of the invention provides a production device and a preparation method of white carbon black, wherein the device comprises the following components: the device comprises a power device, a reaction kettle, a hollow shaft, dispersing blades and a dispersing membrane; the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing membrane are all arranged inside the reaction kettle; the driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate; the dispersing blades are hollow, the hollow shaft is connected with the dispersing blades, and the hollow part of the hollow shaft is communicated with the hollow parts of the dispersing blades; the dispersing blades are provided with air outlet holes communicated with the hollow part inside, the surfaces of the dispersing blades are connected with the dispersing membrane, and one side of the dispersing membrane close to the dispersing blades is communicated with the air outlet holes; the hollow shaft is provided with a shaft gas transmission port, so that gas is transmitted to the hollow shaft, the dispersing blades and the dispersing membrane in sequence through the gas transmission port. Carbon dioxide gas required by producing the white carbon black is dispersed by the dispersion film and then enters the reaction liquid, a special high-pressure pump is not required for conveying, and the dispersed carbon dioxide can be uniformly dispersed in the reaction liquid by utilizing the rotation of the dispersion blade, so that the production of the white carbon black is facilitated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a white carbon black production apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a hollow spindle of the apparatus for producing white carbon black according to the embodiment of the present invention;
FIG. 3 is a schematic top view of a hollow spindle of the apparatus for producing white carbon black according to the embodiment of the present invention;
FIG. 4 is a schematic view of the structure of the portion A-A included in FIG. 2;
fig. 5 is a schematic structural diagram of a white carbon black production apparatus according to an embodiment of the present invention;
fig. 6 is a schematic structural diagram of a dispersion plate in a white carbon black production apparatus according to an embodiment of the present invention;
fig. 7 is a schematic top view of a dispersion plate in a white carbon black production apparatus according to an embodiment of the present invention;
fig. 8 is a schematic flow chart of a method for preparing white carbon black according to an embodiment of the present invention.
Illustration of the drawings:
1-a power plant; 2-a reaction kettle; 3-a hollow shaft;
4-dispersing blades; 5-a dispersion film; 6-a dispersion plate; 7-sealing the box.
Detailed Description
Various embodiments of the present disclosure will be described more fully hereinafter. The present disclosure is capable of various embodiments and of modifications and variations therein. However, it should be understood that: there is no intention to limit the various embodiments of the disclosure to the specific embodiments disclosed herein, but rather, the disclosure is to cover all modifications, equivalents, and/or alternatives falling within the spirit and scope of the various embodiments of the disclosure.
The terminology used in the various embodiments of the present disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the various embodiments of the present disclosure. As used herein, the singular forms are intended to include the plural forms as well, unless the context clearly indicates otherwise. Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the various embodiments of the present disclosure belong. The terms (such as those defined in commonly used dictionaries) should be interpreted as having a meaning that is consistent with their contextual meaning in the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined in various embodiments of the present disclosure.
Example 1
the power device 1 is arranged outside the reaction kettle 2, and the hollow shaft 3, the dispersing blades 4 and the dispersing membrane 5 are all arranged inside the reaction kettle 2;
the driving shaft of the power device 1 is connected with the hollow shaft 3 so as to drive the hollow shaft 3 to rotate;
as shown in fig. 2 to 4, the dispersing blades 4 are hollow inside, the hollow shaft 3 is connected to the dispersing blades 4, and the hollow part of the hollow shaft 3 is communicated with the hollow part of the dispersing blades 4;
the dispersing blades 4 are provided with air outlet holes communicated with the hollow part inside, the surfaces of the dispersing blades 4 are connected with the dispersing membranes 5, and one sides of the dispersing membranes 5 tightly attached to the dispersing blades 4 are communicated with the air outlet holes;
the hollow shaft 3 is provided with a shaft gas transmission port, so that gas is transmitted to the hollow shaft 3, the dispersing blades 4 and the dispersing membrane 5 in sequence through the gas transmission port.
The reaction kettle 2 is used for containing reaction liquid and is a liquid reaction kettle.
The power device 1 is arranged outside the reaction kettle 2 and provides power for the rotation of the hollow shaft 3.
More specifically, the reaction vessel 2 is cylindrical, and the power unit 1 is disposed on a central shaft above the reaction vessel 2.
As shown in fig. 1 or fig. 5, the dispersion blade 4 is driven to rotate by the rotation of the hollow shaft 3, and the hollow structure inside the hollow shaft 3 can transmit gas to the hollow structure of the dispersion blade 4, and the dispersion film 5 on the dispersion blade 4 can disperse other materials to micron level while stirring the liquid, so that the dispersed carbon dioxide is uniformly dispersed in the reaction solution.
Specifically, the hollow shaft 3 may be connected with the dispersing blades 4 at a plurality of positions, so as to form a plurality of layers of dispersing blades 4, thereby achieving a better stirring effect.
The gas enters the dispersing blades 4 from the hollow shaft 3, and the gas is dispersed to reach a micron-sized gas column through the dispersing membrane 5 and directly enters the liquid-solid mixed phase under the rotating state of the dispersing blades 4. Due to the relative operation of the dispersing blades 4 and the mixed liquid, the range of the dispersing blades 4 close to the layer in micron order is uniform and dispersed.
In a specific embodiment, in order to further uniformly disperse the dispersed carbon dioxide in the reaction solution, the apparatus further includes, as shown in fig. 5: a dispersion plate 6; a plate input port is formed in the dispersion plate 6;
as shown in fig. 6-7, the dispersing plate 6 is hollow, and the first surface of the dispersing plate 6 is further provided with an air outlet communicated with the hollow part;
the dispersion film 5 is provided on the first surface of the dispersion plate 6; the other surface of the dispersion plate 6 is fixed on the inner wall of the reaction kettle 2.
Specifically, similar to the dispersing blade 4, the dispersing plate 6 is hollow in the inner structure and is connected with a plate input port so as to be externally connected with input gas, and one surface of the dispersing plate 6 is further provided with a gas outlet communicated with the hollow part in the dispersing plate and communicated to the dispersing membrane 5, so that gas is subjected to dispersing treatment through the dispersing membrane 5, and gas mixing of the reaction liquid is facilitated.
The dispersion plate 6 may be rectangular.
In a specific embodiment, the dispersion film 5 is a multi-layer metal sintered mesh. Specifically, a multilayer metal sintered mesh (for example, 5 layers of metal sintered mesh) can be used as the metal dispersion film, and gas dispersion can be more effectively performed.
Specifically, in a specific embodiment, the filtration precision of the dispersion membrane 5 is any value between 1 and 50 μm, and specifically, for example, the filtration precision may be 1 μm, 2 μm, 3 μm, 5 μm, 7 μm, 10 μm, 15 μm, 17 μm, 20 μm, 22 μm, 23 μm, 25 μm, 27 μm, 30 μm, 35 μm, 37 μm, 40 μm, 45 μm, 47 μm, 50 μm, or the like.
In a specific embodiment, the dispersion membrane 5 is connected to the liquid facing surface of the dispersion blade 4 for better gas dispersion.
In a specific embodiment, the apparatus further comprises: a seal box 7; wherein, the seal box 7 is sleeved on the shaft gas transmission port to ensure the tightness when gas is transmitted to the hollow shaft 3.
Specifically, the sealing box 7 is used for transmitting gas to the hollow shaft 3, so that the gas is not leaked, and the gas tightness is ensured.
In a specific embodiment, in order to accelerate the reaction and increase the solubility of the gas in the terminal portion of the reaction solution, the apparatus may further include: a heater; wherein, the heater is arranged on the reaction kettle 2 and used for heating the reaction kettle 2.
Specifically, in order to facilitate heating, the heater includes: heating wires, or steam coils, or jacketed steam heaters.
In a particular embodiment, the power plant 1 comprises: an electric motor. The rotary power is improved for the hollow shaft 3 by the motor.
Example 2
before the step 101, gas outlets (which may be gas outlets on the dispersion film) are attached to the dispersion blades of the reactor
102, inputting carbon dioxide into the water glass diluent, controlling the reaction temperature range to be between 50 and 90 ℃, and stopping ventilation after the ventilation time is between 5 and 45 min;
specifically, by opening the carbon dioxide valve, carbon dioxide gas can enter the solution obtained in step 101 from the hollow shaft to the dispersing blade (or carbon dioxide gas can be injected into the solution based on the dispersing blade and the dispersing plate together), the reaction temperature is controlled to be 50-90 ℃, the aeration time is controlled to be 5-45min, and the aeration is stopped.
103, continuously introducing carbon dioxide gas into the reaction liquid, controlling the reaction temperature to be 70-95 ℃, and stopping introducing the gas after the gas introducing time is 10-45 min;
specifically, in step 103, carbon dioxide gas is continuously introduced, the reaction temperature is controlled to be 70-95 ℃, the gas introduction time is 10-45min, and the gas introduction is stopped.
and 105, filtering and washing the reaction slurry to obtain a crude product, and pulping and spray-drying the crude product to obtain a nano silicon dioxide product (namely white carbon black).
In a specific embodiment, the water glass diluent in step 101 is prepared by using a sodium silicate solution with a modulus of 2.0-4.0 and a commercial Baume degree of 2-38.
Through the device and the corresponding method of the embodiment of the invention, the nano silicon dioxide is prepared, the nitrogen adsorption specific surface is 180-360 m2/g, the total pore volume is 1.1-2.0 cm3/g, the average pore diameter is 5-25 nm, the median particle size is 1.0-10 μm, and dV/dlogD (the corresponding value at 80nm in nitrogen adsorption data) is less than or equal to 1.8; the product is verified by a rubber formula experiment, and has the advantages of good dispersibility, excellent reinforcing property, low abrasion and good wet skid resistance.
Specifically, the present embodiment may have the following different application examples:
application example 1
The preparation method of the white carbon black in the application example comprises the following steps:
1) the stirring blade of the reaction vessel was equipped with a 1 μm dispersion film.
2) Taking a sodium silicate solution with a modulus of 3.4 and a commercial Baume degree of 38 grade to prepare dilute sodium silicate 120L with a Baume degree of 22;
3) conveying the sodium silicate solution obtained in the step 1) into a 150L reaction kettle through a pump, stirring and heating the liquid, wherein the stirring speed is set to be 12Hz, and the temperature is set to be 70 ℃;
4) when the temperature reaches 70 ℃, opening a carbon dioxide valve, introducing gas into the solution through a hollow shaft and a dispersing blade, introducing carbon dioxide gas with the concentration of 100 wt%, and simultaneously increasing the stirring speed to 20 Hz;
5) introducing carbon dioxide gas for 28min, stopping introducing gas, and setting the temperature at 90 deg.C;
6) when the temperature rises to 90 ℃, the carbon dioxide valve is opened again, carbon dioxide gas with the concentration of 100 wt% is introduced for 17min, and the stirring speed is increased to 38 Hz.
7) Introducing carbon dioxide gas for 115min, stopping introducing gas, simultaneously taking a small amount of reaction liquid, and measuring the pH value of the reaction liquid, wherein the pH value is 8.1;
8) filtering the slurry obtained in the step 7) by using a filter press and washing by using water, and stopping washing when the conductivity of the washing liquid is 1100 mu s/cm, wherein the filter cake is crude silicon dioxide.
9) Pulping the crude product obtained in the step 8), and spray drying to obtain a nano silicon dioxide product.
The product detection indexes are shown in table 1.
Application example 2
The preparation method of the white carbon black in the application example comprises the following steps:
1) the stirring blade of the reaction vessel was equipped with a 5 μm dispersion film.
2) Taking a sodium silicate solution with a modulus of 3.2 and a commercial Baume degree of 38 grade, and preparing dilute water glass 120L with a Baume degree of 25;
3) conveying the sodium silicate solution obtained in the step 2) into a 150L reaction kettle through a pump, starting stirring and heating the liquid, wherein the stirring speed is set to be 12Hz, and the temperature is set to be 70 ℃;
4) when the temperature reaches 70 ℃, opening a carbon dioxide valve, introducing gas into the solution through a hollow shaft and a dispersing blade, introducing carbon dioxide gas with the concentration of 100 wt%, and simultaneously increasing the stirring speed to 20 Hz;
5) introducing carbon dioxide gas for 20min, stopping introducing gas, and setting the temperature at 90 deg.C;
6) when the temperature rises to 90 ℃, the carbon dioxide valve is opened again, carbon dioxide gas with the concentration of 100 wt% is introduced for 25min, and the stirring speed is increased to 38 Hz.
7) Introducing carbon dioxide gas for 110min, stopping introducing gas, simultaneously taking a small amount of reaction liquid, and measuring the pH value of the reaction liquid, wherein the pH value is 8.3;
8) filtering the slurry obtained in the step 7) by using a filter press, washing by using hot water, and stopping washing when the conductivity of the washing liquid is 1100 mu s/cm, wherein the filter cake is crude silicon dioxide.
9) Pulping the crude product obtained in the step 8), and spray drying to obtain a nano silicon dioxide product.
The product detection indexes are shown in table 1.
Application example 3
The preparation method of the white carbon black in the application example comprises the following steps:
1) the stirring blade of the reaction vessel was equipped with a 20 μm dispersion film.
2) Taking a sodium silicate solution with a modulus of 3.3 and a commercial Baume degree of about 38 to prepare dilute sodium silicate 120L with a Baume degree of 16;
3) conveying the sodium silicate solution obtained in the step 2) into a 150L reaction kettle through a pump, stirring and heating the liquid, wherein the stirring speed is set to be 12Hz, and the temperature is set to be 70 ℃;
4) when the temperature reaches 70 ℃, opening a carbon dioxide valve, introducing gas into the solution through a hollow shaft and a dispersing blade, introducing carbon dioxide gas with the concentration of 100 wt%, and simultaneously increasing the stirring speed to 20 Hz;
5) introducing carbon dioxide gas for 20min, stopping introducing gas, and setting the temperature at 90 deg.C;
6) when the temperature rises to 90 ℃, the carbon dioxide valve is opened again, carbon dioxide gas with the concentration of 100 wt% is introduced for 20min, and the stirring speed is increased to 38 Hz.
7) Introducing carbon dioxide gas for 95min, stopping introducing gas, simultaneously taking a small amount of reaction liquid, and measuring the pH value of the reaction liquid, wherein the pH value is 8.3;
8) filtering the slurry obtained in the step 7) by using a filter press, washing by using hot water, and stopping washing when the conductivity of the washing liquid is 1100 mu s/cm, wherein the filter cake is crude silicon dioxide.
9) Pulping the crude product obtained in the step 8), and spray drying to obtain a nano silicon dioxide product.
The product detection indexes are shown in table 1.
Comparative application example 1
The difference from the application example 1 is that the stirring device of the reaction kettle is a stirring paddle for general industry, and the upper end cover of the reaction kettle is provided with a breather pipe device.
The preparation method comprises the following steps:
1) taking a sodium silicate solution with a modulus of 3.4 and a commercial Baume degree of 38 grade to prepare dilute sodium silicate 120L with a Baume degree of 22;
2) conveying the sodium silicate solution obtained in the step 2) into a 150L reaction kettle through a pump, stirring and heating the liquid, wherein the stirring speed is set to be 12Hz, and the temperature is set to be 70 ℃;
3) when the temperature reaches 70 ℃, opening a carbon dioxide valve, introducing gas into the solution, introducing carbon dioxide gas with the concentration of 100 wt%, and simultaneously increasing the stirring speed to 20 Hz;
4) stopping introducing carbon dioxide gas for 160 min;
5) filtering the slurry obtained in the step 4) by using a filter press, washing by using hot water, and stopping washing when the conductivity of the washing liquid is 1100 mu s/cm, wherein the obtained filter cake is crude silicon dioxide.
6) Pulping the crude product obtained in the step 5), and spray drying to obtain a nano silicon dioxide product.
7) The product detection indexes are shown in table 1.
The test data of application examples 1-3, comparative application example 1 for the preparation of nanosilica products are shown in table 1.
TABLE 1 product inspection data for application examples 1-3 and comparative application example 1
Note: 1) nitrogen adsorption specific surface area NSA was determined according to: measuring the total surface area and the external surface area of the carbon black according to GB/T10722-;
2) CTAB specific surface area was determined according to: the specific surface area of the precipitated hydrated silica is determined according to GB/T23656-2009 rubber compounding agent.
3) DBP assay was according to: according to the measurement of the oil absorption value of the precipitated hydrated silica of the HG/T3072-2008 rubber compounding agent.
4) The average pore size was determined according to: GB/T28600 and 2012 rubber compounding agents.
5) dV/dlogD values: nitrogen adsorption data, corresponding to a value at 80 nm.
6) Median particle diameter D50 was determined according to: GB/T32698 2016 rubber compounding agent precipitation hydrated silica particle size distribution determination.
As can be seen from table 1, the scheme corresponding to the present application is significantly superior to the conventional scheme at present, the present invention utilizes the characteristics of the membrane and the gas to disperse the gas membrane to micron level, mixes the gas and the liquid in the reaction vessel through the dispersing blades, and forms local turbulence and micron level laminar flow at the thin surface parallel to the dispersing blades, so that the carbon dioxide can be uniformly dispersed in the solution, and the reaction efficiency can be greatly improved. The method specifically comprises the following steps: the dispersing blades are provided with dispersing membranes, carbon dioxide gas enters the blades from the hollow shaft, and in the rotating state of the dispersing blades, the gas is dispersed by the dispersing membranes and enters a solution after reaching a micron-sized gas column, so that the range of the dispersing blades close to the dispersing membranes is in a micron-sized layer and is uniformly dispersed, the whole solution is in radial flow and axial flow in the reactor, and the reacted slurry is uniformly mixed; furthermore, the invention can reasonably control the carbonization reaction steps, including setting multiple carbonization steps, reasonably controlling the reaction temperature and the ventilation time of each carbonization step, and dispersing the membrane to avoid the problems of equipment blockage and the like.
Those skilled in the art will appreciate that the figures are merely schematic representations of one preferred implementation scenario and that the blocks or flow diagrams in the figures are not necessarily required to practice the present invention.
Those skilled in the art will appreciate that the modules in the devices in the implementation scenario may be distributed in the devices in the implementation scenario according to the description of the implementation scenario, or may be located in one or more devices different from the present implementation scenario with corresponding changes. The modules of the implementation scenario may be combined into one module, or may be further split into a plurality of sub-modules.
The above-mentioned invention numbers are merely for description and do not represent the merits of the implementation scenarios.
The above disclosure is only a few specific implementation scenarios of the present invention, however, the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (10)
1. The utility model provides a white carbon black's apparatus for producing, its characterized in that includes: the device comprises a power device, a reaction kettle, a hollow shaft, dispersing blades and a dispersing membrane;
the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing membrane are all arranged inside the reaction kettle;
the driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate;
the dispersing blades are hollow, the hollow shaft is connected with the dispersing blades, and the hollow part of the hollow shaft is communicated with the hollow parts of the dispersing blades;
the dispersing blades are provided with air outlet holes communicated with the hollow part inside, the surfaces of the dispersing blades are connected with the dispersing membrane, and one side of the dispersing membrane close to the dispersing blades is communicated with the air outlet holes;
the hollow shaft is provided with a shaft gas transmission port, so that gas is transmitted to the hollow shaft, the dispersing blades and the dispersing membrane in sequence through the gas transmission port.
2. The apparatus of claim 1, further comprising: a dispersion plate; a plate input port is formed in the dispersion plate;
the dispersion plate is hollow, and the first surface of the dispersion plate is also provided with an air outlet communicated with the hollow part;
the first surface of the dispersion plate is provided with the dispersion film; the other side of the dispersion plate is fixed on the inner wall of the reaction kettle.
3. The device of claim 1 or 2, wherein the dispersion film is a multi-layer metal sintered mesh.
4. The device according to claim 1 or 2, wherein the dispersion membrane has a filtration precision of between 1 and 50 μm.
5. The apparatus of claim 1, wherein the dispersion membrane is attached to the liquid-facing surface of the dispersion blade.
6. The apparatus of claim 1, further comprising: a sealing box; the sealing box is sleeved on the shaft gas transmission port to ensure the sealing performance when gas is transmitted to the hollow shaft.
7. The apparatus of claim 1, further comprising: a heater; the heater is arranged on the reaction kettle and used for heating the reaction kettle.
8. The apparatus of claim 7, wherein the heater comprises: heating wires, or steam coils, or jacketed steam heaters.
9. A method for preparing white carbon black based on the white carbon black production apparatus of any one of claims 1 to 8, wherein the method comprises:
injecting the water glass diluent into the reaction kettle, and starting a power device to stir and heat;
inputting carbon dioxide into the water glass diluent, controlling the reaction temperature range to be 50-90 ℃, and stopping ventilation after the ventilation time is 5-45 min;
continuously introducing carbon dioxide gas into the reaction solution, controlling the reaction temperature to be 70-95 ℃, and stopping introducing the gas after the introducing time is 10-45 min;
keeping the reaction temperature within the range of 70-95 ℃, starting the power device to stir for 10-150min, and stopping the reaction when the pH value of the reaction solution is controlled to be 5.5-10.0;
and filtering and washing the reaction slurry to obtain a crude product, and pulping and spray-drying the crude product to obtain a nano-silicon dioxide product.
10. The method for preparing white carbon black according to claim 9, wherein the water glass diluent is prepared from a sodium silicate solution with a modulus of 3-4 and a commercial baume degree of 38 grades.
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