CN114634722A - Method for improving structure of regenerated carbon black - Google Patents
Method for improving structure of regenerated carbon black Download PDFInfo
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- CN114634722A CN114634722A CN202210362799.3A CN202210362799A CN114634722A CN 114634722 A CN114634722 A CN 114634722A CN 202210362799 A CN202210362799 A CN 202210362799A CN 114634722 A CN114634722 A CN 114634722A
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- 238000002360 preparation method Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000000576 coating method Methods 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000010058 rubber compounding Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
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-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/482—Preparation from used rubber products, e.g. tyres
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/487—Separation; Recovery
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/60—Agglomerating, pelleting, or the like by dry methods
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
-
- 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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a method for improving a structure of regenerated carbon black, which comprises the steps of carrying out ultrafine grinding on 5-30mm regenerated carbon black coke slag to obtain regenerated carbon black coke slag fine powder with the particle size of 6-45 mu m, putting the regenerated carbon black fine powder into an infiltration tank, introducing steam through a steam pipe, driving a mixing plate to rotate through a driving shaft, mixing, uniformly infiltrating, wherein the degree of wettability before mixing is A, and processing S, F data through a data processing module; the method greatly improves the structure of regenerated carbon black, the reinforcing performance is improved, and fine powder is infiltrated in advance, so that the additional filler has moisture when being mixed and filled, the fine powder is mixed and fully mixed with the fine powder, and meanwhile, after the detection data of the counterclockwise whole pressure detection unit and the clockwise local pressure detection unit are compared with standard data, the mixed humidity change condition can be clearly judged by general detection and sorting, and the humidity is accurately controlled.
Description
Technical Field
The invention relates to the technical field of processing of regenerated carbon black, in particular to a method for improving a structure of the regenerated carbon black.
Background
The regenerated carbon black contains not only the carbon black originally filled in the tire, but also inorganic small materials in the rubber formulation and residues of rubber cracking. The sources and the cracking processes of rubber products are different, the ash content of the regenerated carbon black is different and is in the range of 13-25 wt%, the ash content of the commercial carbon black is only 0.5%, the carbon black has wide application, however, more than 90% of the carbon black is used for reinforcing the rubber, so that the cost of certain rubber products can be greatly reduced if the regenerated carbon black can be applied to the rubber industry, and meanwhile, higher profit can be brought to the cracking industry of waste rubber products;
surface chemistry and surface activity are two important structural parameters of carbon black reinforced rubber, which determine the interaction between carbon black particles and rubber molecules. The specific surface area and the structure degree are two very important parameters for measuring the reinforcing effect of the carbon black on rubber, primary carbon black particles in the industrial carbon black are spherical, the carbon black particles are fused together to form aggregates, the aggregates are similar to grape clusters, the aggregation degree is called the structure degree, and can be measured by a DBP oil absorption value, and the larger the DBP value is, the higher the structure degree is;
the surface active points of the regenerated carbon black are approximately one third of the active points of the carbon black originally filled in the tire, and most of the active points are covered by pyrolysis oil or ash, so that the surface property of the regenerated carbon black is obviously different from that of the commercial carbon black, the activity of the regenerated carbon black is greatly reduced, and the ash is difficult to remove by adopting common physical screening and other processes. How to improve the surface activity and the structure of the thermal cracking carbon black is the biggest difficulty of the project, and the standard of the commercial carbon black is difficult to achieve only by a physical method or a method of adding a modifier.
Disclosure of Invention
The present invention is directed to a method for improving the structure of regenerated carbon black to solve the problems set forth in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method of enhancing the structure of a regenerated carbon black comprising the steps of:
the method comprises the following steps: carrying out ultrafine grinding on the regenerated carbon black coke residue with the particle size of 5-30mm to obtain regenerated carbon black coke residue fine powder with the particle size of 6-45 mu m, and reducing the iron content to 100ppm by two iron removal devices; the coke residue is subjected to superfine grinding, and the particle size is controlled to be 3-45 micrometers so as to reduce the dispersed particle size of the regenerated carbon black in rubber products and improve the performance of the products, and if the particle size is too large, local stress concentration is easily caused to damage the performance of the rubber. And if the content of the organic matters is too small, the aggregation is easy to cause poor dispersion, the ultrafine grinding is favorable for the subsequent oxidation treatment of the oxidant, and because organic matters and ash content are remained in the regenerated carbon black, ozone or hydrogen peroxide is added, and the oxidation corrosion performance of the oxidant is utilized to complete the preliminary reaming of fine micropores in the regenerated carbon black. The treatment time is 10-60min, and the regenerated carbon black with different micropores can be obtained.
Step two: putting the regenerated carbon black fine powder into an infiltration tank, introducing steam through a steam pipe, driving a mixing plate to rotate through a driving shaft, mixing and evenly infiltrating, wherein the infiltration wettability before mixing is A;
step three: the driving shaft is driven by the driving module to rotate in a forward and reverse staggered manner, anticlockwise pressure data S is obtained through detection of the anticlockwise integral pressure detection unit, clockwise local pressure data F is obtained through the clockwise local pressure detection unit, S, F data are processed through the data processing module, and closing time of the steam pipe and opening time of the feeding module are controlled according to the pressure data;
step four: controlling a release unit below the feeding module to be started through the data processing module, feeding an oxidant with the mass ratio of 1-30% of the regenerated carbon black in the feeding module into the infiltration tank for stirring, controlling the temperature of steam infiltration to be 65-100 ℃, and processing for 10-60min to obtain a regenerated carbon black wet material processed by the oxidant, wherein the water content of the regenerated carbon black wet material is 40-60%;
in the continuous steam-introduced atmosphere, part of the fine micropores are burned off to obtain the regenerated carbon black with large pore diameter, so that the regenerated carbon black obtains more fine micropores and larger macropores, and the pore structure and the pore volume of the regenerated carbon black are greatly improved. Under the protection of water vapor, the carbon black cannot burn at high temperature;
step five: conveying the treated wet regenerated carbon black material to an activation furnace, continuously introducing water vapor at the temperature of 650-1000 ℃, and activating for 5-50 min; the surface of the regenerated carbon black after loss of combustion can be exposed to the active points on the surface of partial original carbon black, and a modifier can be added for surface modification. The hydrogen peroxide treatment heating is completed by utilizing the activated waste heat, and the temperature of the discharged regenerated carbon black material is controlled to be 100-200 ℃, so that the surface coating or modification of modifiers such as stearic acid, coupling agents and the like is facilitated;
step six: cooling the activated regenerated carbon black to 100-200 ℃, conveying the regenerated carbon black to a high-speed mixer, and adding a modifier accounting for 0.5-10% of the mass of the regenerated carbon black for modification treatment for 10-60 min;
step seven: and pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree.
As a still further scheme of the invention: step two the mixed plate shape is fence shape, anticlockwise whole pressure detecting element clockwise local pressure detecting element installs respectively the both sides of mixed plate riser, the quantity of mixed plate riser is one at least, the quantity of clockwise local pressure detecting element is two at least.
As a still further scheme of the invention: and step three, the clockwise local pressure detection unit comprises a hemispherical groove arranged on the mixing plate and an elastic membrane sealed at the open end of the hemispherical groove, the inner wall of the elastic membrane is fixedly connected with an elastic unit, two tension detection units are symmetrically arranged in the mixing plate, the end part of the elastic unit is fixedly connected with the detection end of the tension detection unit, and the middle part of the elastic unit is fixedly connected with the elastic membrane through a fixed node.
As a still further scheme of the invention: step three, the data processing module compares the collected values of the anticlockwise overall pressure detection unit and the clockwise local pressure detection unit, and the overall pressure and the local pressure sensed in two directions of the mixing plate are processed through sSign board、sFruit of Chinese wolfberryAnd FSign board、FFruit of Chinese wolfberryComparing and judging the water content of the particles.
As a still further scheme of the invention: the top of the infiltration tank is detachably connected with a control cover, the driving module and the data processing module are installed at the top of the control cover, the steam pipe is provided with a controller which is controlled to be opened and closed by the data processing module, and the bottom of the feeding module is provided with a release unit which is controlled to be opened and closed by the data processing module.
As a still further scheme of the invention: the regenerated carbon black coke residue is one or more of coke residues generated by mixing and cracking waste tires, waste rubber tubes and waste rubber conveying belt rubber products.
As a still further scheme of the invention: the content of the iron in the ultrafine regenerated carbon black powder is reduced to 100ppm by using an impact crusher, a vertical pulverizer or a dry ball mill crushing device, a screening device and an iron removing device in the ultrafine crushing process of the regenerated carbon black.
In a still further embodiment of the present invention, the oxidizing agent is ozone or hydrogen peroxide.
In a still further aspect of the present invention, the modifier is one or more of stearic acid, a silane coupling agent, a phthalate coupling agent, an aluminate coupling agent, a rosin resin, a phenolic resin, a petroleum resin, and a coumarone resin.
Compared with the prior art, the invention has the beneficial effects that:
micropore and macroporous reaming is accomplished to the adoption chemical method, the structure of regeneration carbon black is improved greatly to this method, the reinforcement performance obtains improving, soak the farine in advance simultaneously, thereby make additional filler when the mixture is filled, there is moisture in the farine self, make the mixture of filler and farine more abundant fast, utilize anticlockwise whole pressure detecting element and clockwise local pressure detecting element's detection data and standard data contrast back simultaneously, utilize general examination, the mixed humidity situation of judgement that the sorting can be clear, make humidity obtain accurate control.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
FIG. 1 is a schematic perspective cross-sectional view of an infiltration apparatus for use in a method of enhancing the structure of a regenerated carbon black;
FIG. 2 is a schematic sectional elevation view of one method of enhancing the structure of a regenerated carbon black;
FIG. 3 is an enlarged perspective view of portion A of FIG. 2;
FIG. 4 is a schematic top cross-sectional view of a clockwise partial pressure sensing unit of a method of enhancing the structure of regenerated carbon black;
in the figure: 1. infiltrating the tank; 11. a steam pipe; 12. a controller; 2. a control cover; 3. a drive module; 4. a data processing module; 5. a drive shaft; 51. a mixing plate; 6. a counterclockwise integral pressure detecting unit; 7. a clockwise local pressure detection unit; 71. a hemispherical groove; 72. an elastic film; 73. an elastic unit; 731. a fixed node; 74. a tension detection unit; 8. a feeding module; 81. and releasing the unit.
Detailed Description
Example 1
Selecting regenerated carbon black coke residue obtained by cracking waste tires with the particle size of 5mm as a raw material, carrying out ultrafine crushing by using an impact crusher, reducing the iron content to 100ppm by using two iron removal devices to obtain regenerated carbon black fine powder with the particle size of 6 microns, conveying 100kg of the regenerated carbon black fine powder into a steam infiltration device, introducing steam for infiltration, adding 10kg of hydrogen peroxide with the solid content of 20% for mixing and stirring, controlling the temperature of a roller at 65 ℃, treating for 30min to obtain a hydrogen peroxide treated regenerated carbon black wet material with the water content of 60%, conveying the treated regenerated carbon black wet material into an activation furnace, continuously introducing water vapor at 650 ℃, and activating for 50 min; and cooling the activated regenerated carbon black to 100 ℃, conveying the carbon black to a high-speed mixer, and adding 1kg of modifier Si69 for modification treatment for 10 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.95.
Example 2
Selecting regenerated carbon black coke slag obtained by cracking waste rubber tubes with the particle size of 30mm as a raw material, carrying out ultrafine grinding by using a vertical grinding machine, reducing the iron content to 150ppm by using two iron removal devices to obtain regenerated carbon black fine powder with the particle size of 45 microns, conveying 100kg of the regenerated carbon black fine powder to a steam infiltration device, introducing steam for infiltration, introducing 3kg of ozone for mixing and stirring, controlling the temperature of a roller at 100 ℃, treating for 10min to obtain a hydrogen peroxide treated regenerated carbon black wet material with the water content of 50%, conveying the treated regenerated carbon black wet material to an activation furnace, and continuously introducing steam for activation for 5min at the temperature of 1000 ℃; and cooling the activated regenerated carbon black to 200 ℃, conveying the regenerated carbon black to a steam infiltration device, and adding 5kg of a modifier phthalate coupling agent for modification treatment for 60 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.81.
Example 3
Selecting the regenerated carbon black coke residue obtained by cracking waste tires with the particle size of 25mm as a raw material, carrying out ultrafine crushing by using an impact crusher, reducing the iron content to 120ppm by using two iron removal devices to obtain regenerated carbon black fine powder with the particle size of 18 microns, conveying 100kg of the regenerated carbon black fine powder to a steam infiltration device, introducing steam for infiltration, adding 15kg of hydrogen peroxide with the solid content of 15% for mixing and stirring, controlling the temperature of a roller at 75 ℃, carrying out treatment for 20min to obtain a regenerated carbon black wet material treated by the hydrogen peroxide, wherein the water content is 48%, conveying the treated regenerated carbon black wet material to an activation furnace, continuously introducing water vapor at 850 ℃, and activating for 15 min; and cooling the activated regenerated carbon black to 120 ℃, conveying the regenerated carbon black to a high-speed mixer, and adding 10kg of coumarone resin for modification treatment for 20 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.85.
Example 4
Selecting the regenerated carbon black coke residue obtained by cracking a waste rubber transmission belt with the particle size of 22mm as a raw material, carrying out ultrafine grinding by using a dry ball mill, reducing the iron content to 130ppm by using two iron removal devices to obtain regenerated carbon black fine powder with the particle size of 15 microns, conveying 100kg of the regenerated carbon black fine powder to a steam infiltration device, introducing steam for infiltration, introducing 5kg of ozone for mixing and stirring, controlling the temperature at 80 ℃, treating for 28min to obtain a hydrogen peroxide treated regenerated carbon black wet material with the water content of 52%, conveying the treated regenerated carbon black wet material to an activation furnace, and continuously introducing water vapor at 770 ℃ for activation for 45 min; and cooling the activated regenerated carbon black to 150 ℃, conveying the carbon black to a double-cone mixer, and adding 2kg of modifier stearic acid and 6kg of aminosilane coupling agent for modification treatment for 30 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.88.
Example 5
Selecting the regenerated carbon black coke residue obtained by cracking waste tires with the particle size of 25mm as a raw material, carrying out ultrafine crushing by using an impact crusher, reducing the iron content to 110ppm by using two deironing devices to obtain regenerated carbon black fine powder with the particle size of 22 mu m, conveying 100kg of the regenerated carbon black fine powder to a steam infiltration device, introducing steam for infiltration, adding 5kg of hydrogen peroxide with the solid content of 12%, mixing and stirring, controlling the temperature of a roller at 75 ℃, treating for 40min to obtain a regenerated carbon black wet material treated by the hydrogen peroxide, wherein the water content is 50%, conveying the treated regenerated carbon black wet material to an activation furnace, continuously introducing water vapor at 680 ℃, and activating for 50 min; and cooling the activated regenerated carbon black to 140 ℃, conveying the regenerated carbon black to a high-speed mixer, and adding 1kg of modifier Si69 and 6kg of petroleum resin for modification treatment for 15 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.92.
Example 6
Selecting the regenerated carbon black coke residue obtained by cracking waste tires with the particle size of 24mm as a raw material, carrying out ultrafine crushing by using a ring roller crusher, reducing the iron content to 100ppm by using two iron removal devices to obtain regenerated carbon black fine powder with the particle size of 6 microns, conveying 100kg of the regenerated carbon black fine powder to a steam infiltration device, introducing steam for infiltration, adding 22kg of 15% solid content hydrogen peroxide for mixing and stirring, controlling the temperature of a roller at 76 ℃ for 34min, obtaining a regenerated carbon black wet material treated by the hydrogen peroxide, wherein the water content is 53%, conveying the treated regenerated carbon black wet material to an activation furnace, continuously introducing water vapor at 830 ℃, and activating for 17 min; and cooling the activated regenerated carbon black to 150 ℃, conveying the regenerated carbon black to a steam infiltration device, and adding 1kg of modifier phthalate coupling agent and 3kg of stearic acid for modification treatment for 18 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.98.
Example 7
Selecting regenerated carbon black coke slag obtained by cracking waste rubber tubes with the particle size of 8mm as a raw material, carrying out ultrafine crushing by using an impact crusher, reducing the iron content to 155ppm by using two iron removal devices to obtain regenerated carbon black fine powder with the particle size of 25 mu m, conveying 100kg of the regenerated carbon black fine powder to a steam infiltration device, introducing steam for infiltration, introducing 10kg of ozone for mixing and stirring, controlling the temperature of a roller at 68 ℃, treating for 44min to obtain a hydrogen peroxide treated regenerated carbon black wet material with the water content of 51%, conveying the treated regenerated carbon black wet material to an activation furnace, and continuously introducing steam for 34min under the condition of 720 ℃; and cooling the activated regenerated carbon black to 150 ℃, conveying the carbon black to a double-cone mixer, and adding 1kg of modifier Si75 and 5kg of stearic acid for modification treatment for 25 min. And pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree, wherein the oil absorption value is 0.86.
Example 8
This example is specifically described in comparative examples 1 to 3.
Comparative example 1 provides a method of preparation of regeneration, reference example 1, except that: the difference lies in that: only step 1.
Step 1 of comparative example 1 was: after the superfine grinding is carried out by adopting an impact crusher, the content of iron is reduced to 100ppm by two iron removal devices, and the regenerated carbon black fine powder with the particle size of 6 mu m is obtained.
Comparative example 2
Comparative example 2 provides a regenerated preparation method, reference example 1, with the difference that: steps 5,6 and 7 are absent and the remaining steps are the same.
Comparative example 3
Comparative example 3 provides a method for preparing ultra-fine cracked carbon black, with reference to example 1, except that: steps 6 and 7 are omitted and the remaining steps are the same.
Comparative example 1
In order to comparatively illustrate the influence of the regenerated carbon blacks obtained in different examples and comparative examples on the rubber performance, the mechanical properties and the like of the rubber were measured after the regenerated carbon blacks of different examples and comparative examples were applied to the rubber according to the following methods, and the test results are shown in table 1.
The concrete rubber material is prepared by mixing the following components in parts by weight: 100 parts of Natural Rubber (NR), 50 parts of regenerated carbon black in examples and comparative examples, 5.0 parts of zinc oxide, 3.0 parts of stearic acid, 0.6 part of accelerator DM and 2.5 parts of sulfur.
TABLE 1 results of testing the Properties of different rubbers
Referring to fig. 1, 2, 3, and 4, in the embodiment of the present invention of steam infiltration wettability control, in order to improve the mixing efficiency, the fine powder is in a dry state before being subjected to steam infiltration, and steam infiltration is a process, so the steam infiltration is set to two steps, the first step is fine powder pre-infiltration, the second step is mixed infiltration, the degree of wetting before mixing is set to a, the humidity of pre-infiltrated particles is less than 40%, since the gravity of the regenerated carbon black coke residue fine powder increases after the humidity of the regenerated carbon black coke residue fine powder increases, when stirring and rotating, the contact pressure to the mixing plate 51 is different when the humidity of carbon black coke residue fine powder with different humidity changes, and thus the basis for humidity judgment is provided;
firstly, according to the humidity requirement and different implementation methods, a plurality of groups of carbon black coke residue fine powder with standard humidity are set, the humidity of the carbon black coke residue fine powder is controlled to be the soaking degree A before mixing, at the moment, the first soaking degree A is put into the soaking tank 1, the control cover 2 is closed, the driving module 3 rotates to drive the clockwise local pressure detection unit 7 to rotate in the forward and reverse directions, at the moment, when the mixing plate 51 rotates anticlockwise, the anticlockwise integral pressure detection unit 6 is an integral pressure detection mechanism, at the moment, the anticlockwise integral pressure detection unit 6 collects the carbon black coke residue fine powder with the soaking degree A before mixing to rotate anticlockwiseThe overall pressure of the overall pressure detecting unit 6, and when the mixing plate 51 rotates clockwise, the pressure s against the particles at the time of rotation of the carbon black char fine powder of the pre-mixing immersion wettability A detected by the clockwise partial pressure detecting unit 7 is obtainedSign boardWhen the mixing plate 51 rotates clockwise, the particles will be subjected to a reaction force, the elastic membrane 72 deforms elastically in the hemispherical groove 71 and bends inward, the fixing node 731 drives the elastic unit 73 to deform elastically, and the tension detection unit 74 detects a pressure FSign boardComparing with a vertical direction of one mixing plate 51 as a group, a plurality of s are collectedSign boardAnd FSign boardThe standard numerical value is obtained, the interior of the driving shaft 5 is of a hollow structure, and data transmission lines of the anticlockwise integral pressure detection unit 6 and the clockwise local pressure detection unit 7 penetrate through the driving shaft 5 to be in signal connection with the data processing module 4, so that the driving shaft 5 adopts a forward and reverse rotation mode to avoid the circuit from being twisted, and meanwhile, the forward and reverse rotation can adopt double-sided pressure detection to judge the particle conditions on the front side and the rear side of the fan blade;
the number of the clockwise partial pressure detecting units 7 is several, in order to further improve the accuracy of the detection, since the counterclockwise overall pressure detecting unit 6 is integrated, the humidity of the upper particles is 60% and the humidity of the lower particles is 20% in the particles in front of the counterclockwise overall pressure detecting unit 6, and the weight influence caused by the upper particle humidity and the lower particle humidity is consistent with the weight influence of the uniformly distributed particles of 40 percent, when the clockwise local pressure detection unit 7 rotates clockwise, the clockwise local pressure detection units 7 which are vertically distributed can respectively detect the humidity of the longitudinally distributed particles to change the particles into local detection, by combining the clockwise local pressure detection unit 7 with the anticlockwise overall pressure detection unit 6 and mutually correcting, more accurate humidity condition can be obtained;
at this time, when the data processing module 4 reaches the data standard of the immersion wettability A before mixing according to the data condition detected by the counterclockwise integral pressure detecting unit 6, the releasing unit 81 at the bottom of the feeding module 8 is controlled to be opened, and at this time, the feeding module 8 rotates synchronously with the rotation of the driving shaft 5 and is uniformly sprayed on the data standardThe fine powder is mixed twice, and s detected by the counterclockwise integral pressure detecting unit 6 is continuedFruit of Chinese wolfberryAnd pressure after mixing sSign boardF detected by the clockwise local pressure detection unit 7Fruit of Chinese wolfberryAnd post-mixing pressure FSign boardComparing until the actual numerical value meets the standard numerical value, closing the controller 12 on the steam pipe 11 through the data processing module 4 to complete mixing, wherein a plurality of steam infiltration devices can be arranged according to the type of added additional filler, for example, when auxiliary gas is added, the feeding module 8 is replaced by a gas supply pipeline arranged at the other side of the infiltration tank 1;
this mode can be soaked the farine in advance to make additional filler when the mixture is filled, there is moisture in farine self, makes the mixture of filler and farine more quick abundant, utilizes anticlockwise whole pressure detection unit 6 and clockwise local pressure detection unit 7's detection data and standard data contrast back simultaneously, utilizes general examination, go out the judgement mixing humidity situation that can be clear separately, makes humidity obtain accurate control.
From the test results, the regenerated carbon black product prepared by the scheme of the invention has relatively improved reinforcing performance, is close to the reference carbon black sold in the market, and can partially or completely replace the reference carbon black sold in the market. The regenerated carbon black treated by the technology has excellent compatibility with rubber, can promote the reinforcing effect of the regenerated carbon black, improve various performances of rubber materials, realize effective resource recycling, improve the additional value of effective resources and reduce the cost of the rubber industry.
From the test results, the regenerated carbon black product prepared by the scheme of the invention has relatively improved reinforcing performance, is close to the reference carbon black sold in the market, and can partially or completely replace the reference carbon black sold in the market. The regenerated carbon black treated by the technology has excellent compatibility with rubber, can promote the reinforcing effect of the regenerated carbon black, improve various performances of rubber materials, realize effective resource recycling, improve the added value of effective resources and reduce the cost of the rubber industry.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (9)
1. A method for improving the structure of regenerated carbon black, which is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: carrying out ultrafine grinding on the regenerated carbon black coke residue with the particle size of 5-30mm to obtain regenerated carbon black coke residue fine powder with the particle size of 6-45 mu m, and reducing the iron content to 100ppm by two iron removal devices;
step two: putting the regenerated carbon black fine powder into the infiltration tank (1), introducing steam through a steam pipe (11), driving a mixing plate (51) to rotate through a driving shaft (5), mixing and infiltrating uniformly, wherein the infiltration wettability before mixing is A;
step three: the driving shaft (5) is driven to rotate in a forward and reverse staggered manner through the driving module (3), counterclockwise pressure data S is obtained through detection of the counterclockwise integral pressure detection unit (6), clockwise local pressure data F is obtained through the clockwise local pressure detection unit (7), S, F data are processed through the data processing module (4), and the closing time of the steam pipe (11) and the opening time of the feeding module (8) are controlled according to the pressure data;
step four: controlling a release unit (81) below the feeding module (8) to be started through the data processing module (4), feeding an oxidant with the mass ratio of 1-30% of the regenerated carbon black in the feeding module (8) into the infiltration tank (1) for stirring, controlling the temperature of steam infiltration to be 65-100 ℃, and processing for 10-60min to obtain a regenerated carbon black wet material processed by the oxidant, wherein the water content is 40-60%;
step five: conveying the treated wet regenerated carbon black material to an activation furnace, continuously introducing water vapor at the temperature of 650-1000 ℃, and activating for 5-50 min;
step six: cooling the activated regenerated carbon black to 100-200 ℃, conveying the regenerated carbon black to a high-speed mixer, and adding a modifier accounting for 0.5-10% of the mass of the regenerated carbon black for modification treatment for 10-60 min;
step seven: and pressing the modified regenerated carbon black into particles by using dry granulation equipment to obtain the regenerated carbon black with high structure degree.
2. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: step two the mixed plate (51) shape is fence shape, anticlockwise whole pressure detecting element (6), clockwise local pressure detecting element (7) install respectively the both sides of mixed plate (51) riser, the quantity of mixed plate (51) riser is one at least, the quantity of clockwise local pressure detecting element (7) is two at least.
3. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: step three clockwise local pressure detecting element (7) including set up hemisphere groove (71) on mixing plate (51) and seal and be in hemisphere groove (71) open end's elastic membrane (72), the inner wall fixedly connected with elasticity unit (73) of elastic membrane (72), two pulling force detecting element (74) are installed to symmetry in mixing plate (51), the tip of elasticity unit (73) with pulling force detecting element (74) detection end fixed connection, the middle part of elasticity unit (73) pass through fixed node (731) with elastic membrane (72) fixed connection.
4. The method of claim 2, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: thirdly, the data processing module (4) compares the collected values of the anticlockwise overall pressure detection unit (6) and the clockwise local pressure detection unit (7), and the overall pressure and the local pressure sensed in two directions of the mixing plate (51) are processed through sSign board、sFruit of Chinese wolfberryAnd FSign board、FFruit of Chinese wolfberryComparing and judging the water content of the particles.
5. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: the top of infiltration jar (1) is dismantled and is connected with control lid (2), drive module (3) data processing module (4) are installed the top of control lid (2), install on steam pipe (11) through controller (12) that data processing module (4) control was opened and close, throw the bottom of material module (8) and install release unit (81) that data processing module (4) control was opened and close.
6. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: the regenerated carbon black coke residue is one or more of coke residues generated by mixing and cracking waste tires, waste rubber tubes and waste rubber conveying belt rubber products.
7. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: in the process of ultrafine grinding of the regenerated carbon black, an impact crusher, a vertical mill or a dry ball mill grinding device is selected, a screening device and an iron removal device are selected to reduce the iron content of the ultrafine regenerated carbon black powder to 100 ppm.
8. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: the oxidant is ozone or hydrogen peroxide.
9. The method of claim 1, wherein the step of increasing the structure of the regenerated carbon black comprises the steps of: the modifier is one or more of stearic acid, silane coupling agent, phthalate coupling agent, aluminate coupling agent, rosin resin, phenolic resin, petroleum resin and coumarone resin.
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