CN112194171A - Novel process for reducing ash content of pyrolysis carbon black and recovering beneficial components - Google Patents
Novel process for reducing ash content of pyrolysis carbon black and recovering beneficial components Download PDFInfo
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- 239000006229 carbon black Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 52
- 230000008569 process Effects 0.000 title claims abstract description 51
- 230000009286 beneficial effect Effects 0.000 title claims abstract description 27
- 238000000197 pyrolysis Methods 0.000 title claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 18
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 15
- 239000010959 steel Substances 0.000 claims abstract description 15
- 238000005188 flotation Methods 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 33
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 19
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 14
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 11
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 11
- 229960001763 zinc sulfate Drugs 0.000 claims description 11
- TUZCOAQWCRRVIP-UHFFFAOYSA-N butoxymethanedithioic acid Chemical compound CCCCOC(S)=S TUZCOAQWCRRVIP-UHFFFAOYSA-N 0.000 claims description 7
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 6
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 6
- 239000005083 Zinc sulfide Substances 0.000 claims description 6
- 239000004571 lime Substances 0.000 claims description 6
- 239000006148 magnetic separator Substances 0.000 claims description 6
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000003607 modifier Substances 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000007885 magnetic separation Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 241000565357 Fraxinus nigra Species 0.000 claims 3
- 238000004064 recycling Methods 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 35
- 239000010920 waste tyre Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000005406 washing Methods 0.000 description 5
- 241000872198 Serjania polyphylla Species 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052950 sphalerite Inorganic materials 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 125000003636 chemical group Chemical group 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 125000000686 lactone group Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 125000004151 quinonyl group Chemical group 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000006235 reinforcing carbon black Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
-
- 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
- C09C1/56—Treatment of carbon black ; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a new process for reducing ash content of pyrolysis carbon black and recovering beneficial components, belonging to the technical field of waste tire treatment; through the re-drying process, the problem that size mixing is difficult is solved while oil content is recovered. The invention has simple process flow and low implementation cost. The ash content of the cracking carbon black is reduced, and the surface activity of the cracking carbon black is improved; can recover steel wires, oil and ZnS, and create economic benefit.
Description
Technical Field
The invention belongs to the technical field of waste tire treatment, and particularly relates to a novel process for reducing ash content of pyrolysis carbon black and recovering beneficial components.
Background
After the waste tires are processed by a thermal cracking process, steel wires, cracking oil, cracking carbon black and noncondensable gas are generated, wherein the proportion of the cracking carbon black can reach about 35%, but the cracking carbon black can not be directly used as industrial carbon black again: the graphite microcrystal surface of the industrial carbon black has defects, and the edge of the graphite microcrystal has a certain amount of chemical groups such as free radicals, hydroxyl groups, lactone groups, carboxyl groups, quinone groups and the like, and the chemical groups with higher surface activity can react with rubber macromolecular chain free radicals generated by shearing and thermal induction in the mixing process to increase the interaction force between the carbon black and the polymer molecular chain and improve the reinforcing effect. In the thermal cracking process of the waste tire, the original active site of the carbon black is covered by ash and a small amount of macromolecular rubber hydrocarbon chains (pyrolysis oil), namely, carbonaceous deposits, so that the surface activity is reduced, and therefore, the waste tire pyrolysis carbon black has an inert surface, so that the reinforcing effect of the waste tire pyrolysis carbon black on rubber is poor. Therefore, the ash content and the carbonaceous sediment of the cracked carbon black are reasonably and effectively removed, and the method has a promoting effect on the resource utilization of the waste tires.
The ash content of the pyrolysis carbon black mainly consists of zinc-containing inorganic additives and white carbon black (SiO 2). Due to the difference of the previous cracking process, the inorganic component additive ZnO is uniformly attached to the surface of the cracked carbon black in the form of ZnS. Therefore, it is of great significance to develop a process that can reduce the ash content of the cracked carbon black and effectively recover ZnS.
Patent No. 102504619B discloses a purification process of carbon black, especially a purification process of carbon black from waste tire cracking, which comprises acid washing and alkali washing, wherein the carbon black after acid washing and alkali washing is subjected to acid washing again. According to the purification process, the ash content of the carbon black is reduced from 18.7% to 2.6%, the volatile matter is reduced from 9.5% to 5.0%, but a large amount of acid and alkali chemicals are consumed; the equipment maintenance and waste liquid treatment cost is high; and beneficial components ZnS in oil and ash are not recovered.
Patent No. 109054464a discloses a tire cracking carbon black physical deliming process, but the ash content is reduced by about 5%, the yield is only 55%, and the tailings after flotation still need to be treated; and beneficial components ZnS in oil and ash are not recovered.
Disclosure of Invention
The invention aims to provide a novel process for reducing ash content of cracking carbon black and recovering beneficial components, and aims to solve the technical problems that the cracking carbon black of a waste tire has an inert surface and the rubber reinforcing effect is poor.
In order to achieve the purpose, the specific technical scheme of the novel process for reducing the ash content of the cracking carbon black and recovering beneficial components is as follows:
1. separating and recovering residual and doped fine steel wires in the cracking carbon black by a magnetic separator (with Gaussian intensity of 8000);
2. heating and drying the cracked carbon black subjected to magnetic separation for 30-60 min by using a hot-blast stove, wherein the drying temperature is 180-220 ℃; the volatile content is 2-8%, and the volatile content comprises oil gas and non-condensable gas; collecting oil through a condensing device;
3. grinding the dried cracked carbon black to 300 meshes which account for 90 percent, and then carrying out flotation;
4. and a small amount of surface modifier such as ethanol is used to further enhance the surface hydrophilicity of the carbon black. Adopting a carbon black preferential flotation process, wherein the flotation parameters are as follows: the concentration of the slurry is 5 to 20 percent; the flotation temperature is room temperature;
5. the cracking carbon black roughing process comprises the following steps: the size mixing time is 20-40 s, zinc sulfate (300-600 g/t) and sodium sulfite (300-600 g/t) are added to inhibit the zinc sulfate, and the stirring time is 3-5 min; adding 10-20 g/t of 2# oil after stirring, wherein the stirring time is 0.5-2 min, and the flotation time is 2-5 min;
6. the selection process of the cracking carbon black comprises the following steps: the concentration of the slurry is 5-15%, the slurry mixing time is 0.5-1 min, 2# oil (3-10 g/t) is added, the flotation time is 2-5 min, and the middle sample returns to the rough concentration;
7. the zinc sulfide roughing process comprises the following steps: the flotation concentration of a cracked carbon black roughing tail sample is 30-50%, the size mixing time is 20-40 s, lime is added, the pH value is adjusted to 10-11, activating agent copper sulfate (100-200 g/t) is added for activation, the stirring time is 2-5 min, butyl xanthate (100-200 g/t) is added, the stirring time is 1-3 min, 2# oil (50-70 g/t) is added, the stirring time is 0.5-1 min, and the flotation time is 2-5 min;
8. and (5) filtering and drying.
According to the invention, through a re-drying process, the problem of difficult size mixing is solved while oil content is recovered;
SiO2 has strong hydrophilicity, zinc sulfate and sodium sulfite can effectively inhibit ZnS, and cracked carbon black can be separated from ZnS and SiO 2; the copper sulfate can activate the ZnS, and then the ZnS is collected by the butyl xanthate, so that the aim of enriching and recovering the beneficial component ZnS is fulfilled.
The novel process for reducing the ash content of the pyrolysis carbon black and recovering beneficial components has the following advantages: effectively recovering fine steel wires in the cracked carbon black; the oil content of the cracking carbon black is reduced, and the pungent smell is eliminated; the surface activity of the pyrolysis carbon black is improved, the ash content of the pyrolysis carbon black is reduced, and simultaneously the beneficial component ZnS in the ash content is recovered; the process flow is simple and the implementation cost is low. The ash content of the cracking carbon black is reduced, and the surface activity of the cracking carbon black is improved; can recover steel wires, oil and ZnS, and create economic benefit.
Drawings
FIG. 1 is a flow diagram of a novel process of the present invention for reducing the ash content of cracked carbon black and for recovering beneficial components.
Detailed Description
For a better understanding of the objects, structure and function of the invention, a novel process for the reduction of ash content and recovery of beneficial components of cracked carbon black of the present invention is described in further detail below with reference to the accompanying drawings.
As shown in figure 1, the cracked carbon black still contains 0.2 to 3 percent of steel wires due to the difference of the tire treatment process at the early stage of cracking. According to the process, the steel wire is efficiently recycled through a magnetic separator with the magnetic field intensity of 8000 Gauss, so that the appearance, the dispersity and the aging property of final products (pigment carbon black, reinforcing carbon black and the like) of the cracking carbon black are improved while the subsequent deep processing production is facilitated. The different cracking processes result in 1% -8% of the cracking oil (macromolecular rubber hydrocarbon chain) attached to the surface of the cracking carbon black, and are accompanied by various degrees of pungent odor, wherein the pungent odor is mainly caused by the non-completely volatilized cracking oil. The re-volatilization not only reduces the smell, but also condenses the volatilized oil content, and can recover the oil content again for sale. Heating the cracked carbon black to a proper temperature, and condensing and recovering oil components volatilized again on the surface of the cracked carbon black, so that benefits are created;
the pyrolysis oil covering the active sites can be removed by heating and drying again, but the pyrolysis carbon black is agglomerated due to the rapid volatilization of oil components due to rapid temperature rise, so that the particle size is uneven, and the surface activity is reduced. Grinding the carbon black powder to a certain particle size range can improve the surface activity of the cracked carbon black and is beneficial to the subsequent ash reduction process. The hydrophilicity of the cracked carbon black after surface oil removal is enhanced, and uniform and stable slurry is easily formed under the slurry mixing and dispersing effects of flotation equipment. According to the surface characteristic difference of the carbon black, ZnS and SiO2, selecting proper medicaments to effectively separate the carbon black, ZnS and SiO2, so that the ash content of the cracked carbon black is reduced from 18.2% to 7.8%, and the yield is 82.9%; the cycle yield of the intermediate sample is 3.9%; the beneficial component ZnS is recovered, the yield is 7.1 percent, and the ZnS content is 59 percent; the tailing yield was 6.1%.
Example 1:
1. separating and recovering residual and doped fine steel wires in the cracking carbon black by a magnetic separator (with Gaussian intensity of 8000);
2. heating and drying the magnetic separated pyrolysis carbon black for 45min by a hot blast stove, wherein the drying temperature is 200 ℃; the volatile component content is 2-8% (no clear value exists because the volatile component contents of the cracking carbon black produced by different cracking processes) and comprises oil gas and non-condensable gas; collecting oil through a condensing device;
3. grinding the dried cracked carbon black to 300 meshes which account for 90 percent, and then carrying out flotation;
4. and a small amount of surface modifier such as ethanol is used to further enhance the surface hydrophilicity of the carbon black. Adopting a carbon black preferential flotation process, wherein the flotation parameters are as follows: the slurry concentration is 10%; the flotation temperature is room temperature;
5. the cracking carbon black roughing process comprises the following steps: the size mixing time is 30s, zinc sulfate (400g/t) and sodium sulfite (350g/t) are added to inhibit the zinc sulfate, and the stirring time is 4.5 min; adding 2# oil (150g/t) after stirring, wherein the stirring time is 1min, and the flotation time is 4 min;
6. the selection process of the cracking carbon black comprises the following steps: the concentration of the slurry is 5%, the slurry mixing time is 0.5min, 2# oil (5g/t) is added, the flotation time is 3.5min, and the medium sample is returned to the roughing;
7. the zinc sulfide roughing process comprises the following steps: the flotation concentration of a cracked carbon black roughing tail sample is 40%, the size mixing time is 30s, lime is added, the pH value is adjusted to 10-11, an activator copper sulfate (150g/t) is added for activation, the stirring time is 3min, butyl xanthate (150g/t) is added, the stirring time is 2.5min, No. 2 oil (60g/t) is added, the stirring time is 0.5min, and the flotation time is 3.5 min;
8. filtering and drying to obtain the cracked carbon black with ash content of 7.8 percent and yield of 82.9 percent; recovering 0.2-3% of steel wires; recovering 2-8% of oil; the content of ZnS which is a beneficial component is recovered to be 59 percent, and the yield is 7.1 percent; the tailing yield was 6.1%.
And (3) performance testing:
cracked carbon black with ash of 7.8% and yield of 82.9%; recovering 0.2-3% of steel wires; recovering 2-8% of oil; the content of ZnS which is a beneficial component is recovered to be 59 percent, and the yield is 7.1 percent; the tailing yield was 6.1%.
Example 2:
1. separating and recovering residual and doped fine steel wires in the cracking carbon black by a magnetic separator (with Gaussian intensity of 8000);
2. heating and drying the magnetic separated pyrolysis carbon black for 45min by a hot blast stove, wherein the drying temperature is 200 ℃; the volatile content is 2-8%, and the volatile content comprises oil gas and non-condensable gas; collecting oil through a condensing device;
3. grinding the dried cracked carbon black to 300 meshes which account for 90 percent, and then carrying out flotation;
4. and a small amount of surface modifier such as ethanol is used to further enhance the surface hydrophilicity of the carbon black. Adopting a carbon black preferential flotation process, wherein the flotation parameters are as follows: the slurry concentration is 5%; the flotation temperature is room temperature;
5. the cracking carbon black roughing process comprises the following steps: the size mixing time is 20s, zinc sulfate (300g/t) + sodium sulfite (300g/t) is added to inhibit the zinc sulfate, and the stirring time is 3 min; adding 2# oil (10g/t) after stirring, wherein the stirring time is 0.5min, and the flotation time is 2 min;
6. the selection process of the cracking carbon black comprises the following steps: the concentration of the slurry is 5%, the slurry mixing time is 0.5min, 2# oil (3g/t) is added, the flotation time is 2min, and the medium sample returns to the rough concentration;
7. the zinc sulfide roughing process comprises the following steps: the flotation concentration of a cracked carbon black roughing tail sample is 30%, the size mixing time is 20s, lime is added, the pH value is adjusted to 10-11, an activator copper sulfate (100g/t) is added for activation, the stirring time is 2min, butyl xanthate (100g/t) is added, the stirring time is 1min, 2# oil (50g/t) is added, the stirring time is 0.5min, and the flotation time is 2 min;
8. and (5) filtering and drying.
And (3) performance testing:
cracked carbon black with 11.6% ash and 90.1% yield; recovering 0.2-3% of steel wires; recovering 2-8% of oil; the content of ZnS which is a beneficial component is recovered to be 21 percent, and the yield is 8.2 percent; the tailing yield was 1.7%.
Example 3:
1. separating and recovering residual and doped fine steel wires in the cracking carbon black by a magnetic separator (with Gaussian intensity of 8000);
2. heating and drying the magnetic separated pyrolysis carbon black for 45min by a hot blast stove, wherein the drying temperature is 200 ℃; the volatile content is 2-8%, and the volatile content comprises oil gas and non-condensable gas; collecting oil through a condensing device;
3. grinding the dried cracked carbon black to 300 meshes which account for 90 percent, and then carrying out flotation;
4. and a small amount of surface modifier such as ethanol is used to further enhance the surface hydrophilicity of the carbon black. Adopting a carbon black preferential flotation process, wherein the flotation parameters are as follows: the slurry concentration is 20%; the flotation temperature is room temperature;
5. the cracking carbon black roughing process comprises the following steps: the size mixing time is 40s, zinc sulfate (600g/t) and sodium sulfite (600g/t) are added to inhibit the zinc sulfate, and the stirring time is 5 min; adding 10-20 g/t of 2# oil after stirring, wherein the stirring time is 2min, and the flotation time is 5 min;
6. the selection process of the cracking carbon black comprises the following steps: the concentration of the slurry is 15%, the slurry mixing time is 1min, 2# oil (10g/t) is added, the flotation time is 5min, and the medium sample returns to the rough concentration;
7. the zinc sulfide roughing process comprises the following steps: the flotation concentration of a cracked carbon black roughing tail sample is 50%, the size mixing time is 40s, lime is added, the pH value is adjusted to 10-11, an activator copper sulfate (200g/t) is added for activation, the stirring time is 5min, butyl xanthate (200g/t) is added, the stirring time is 3min, 2# oil (70g/t) is added, the stirring time is 1min, and the flotation time is 5 min;
8. and (5) filtering and drying.
And (3) performance testing:
cracked carbon black with 11.5% ash and 89.7% yield; recovering 0.2-3% of steel wires; recovering 2-8% of oil; the content of ZnS which is a beneficial component is recovered to be 34 percent, and the yield is 6.2 percent; the tailing yield was 4.1%.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (8)
1. A novel process for reducing ash content of cracked carbon black and recovering beneficial components is characterized by comprising the following steps which are carried out in sequence;
s1, separating and recycling the fine steel wires by the cracked carbon black through a magnetic separator;
s2, heating and drying the cracked carbon black subjected to magnetic separation by a hot blast stove, and collecting oil components by a condensing device;
s3, grinding and floating the dried cracked carbon black in the S2;
step S4, a cracked carbon black roughing process, namely, firstly adding zinc sulfate and sodium sulfite, stirring and mixing, then adding No. 2 oil, stirring for a moment, and then carrying out flotation;
s5, carrying out a concentration process of the cracked carbon black, controlling the concentration of the slurry to be 5-15%, adding No. 2 oil again, carrying out flotation, and returning the medium sample to rough concentration;
step S6, a zinc sulfide roughing process, adding lime, adjusting pH to mix slurry, adding an activator copper sulfate to activate, reacting for a period of time, adding butyl xanthate and No. 2 oil, stirring, and performing flotation;
and S7, filtering and drying.
2. The novel process for reducing ash content of pyrolysis carbon black and recovering beneficial components, according to claim 1, is characterized in that in the step S2, the pyrolysis carbon black after magnetic separation is heated and dried for 30-60 min by a hot blast stove, and the drying temperature is 180-220 ℃; the volatile content is 2-8%, and the volatile content comprises oil gas and non-condensable gas; the oil is collected by a condensing device.
3. The novel process for reducing ash content in cracked carbon black and recovering beneficial components as claimed in claim 1, wherein in step S3, after grinding to 300 mesh 90%, flotation is performed.
4. The novel process for reducing ash content in cracked carbon black and recovering beneficial components as claimed in claim 3, wherein said step S3' includes adding surface modifier to the ground material obtained in said step S3, and then subjecting the ground material to flotation.
5. The novel process for reducing ash content of cracked carbon black and recovering beneficial components as claimed in claim 4, wherein in step S3', flotation is performed with carbon black and the slurry concentration is 5% -20%; the flotation temperature was room temperature.
6. The novel process for the reduction of cracked carbon black ash and the recovery of beneficial components as claimed in claim 1, wherein step S4, cracked carbon black rougher process: the size mixing time is 20-40 s, zinc sulfate (300-600 g/t) and sodium sulfite (300-600 g/t) are added, and the stirring time is 3-5 min; and adding 10-20 g/t of 2# oil after stirring, wherein the stirring time is 0.5-2 min, and the flotation time is 2-5 min.
7. The novel process for the reduction of cracked carbon black ash and the recovery of beneficial components as claimed in claim 1, wherein step S5, cracked carbon black beneficiation process: the concentration of the slurry is 5-15%, the slurry mixing time is 0.5-1 min, 2# oil (3-10 g/t) is added, the flotation time is 2-5 min, and the medium sample returns to the rough concentration.
8. The novel process for the reduction of cracked carbon black ash and the recovery of beneficial components as claimed in claim 1, wherein step S6, zinc sulfide rougher process: the flotation concentration of a cracked carbon black roughing tailing sample is 30-50%, the size mixing time is 20-40 s, lime is added, the pH value is adjusted to 10-11, activating agent copper sulfate (100-200 g/t) is added for activation, the stirring time is 2-5 min, butyl xanthate (100-200 g/t) is added, the stirring time is 1-3 min, 2# oil (50-70 g/t) is added, the stirring time is 0.5-1 min, and the flotation time is 2-5 min.
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| CN113563743A (en) * | 2021-07-09 | 2021-10-29 | 中国化学工业桂林工程有限公司 | A kind of catalytic regeneration method of cracking carbon black |
| CN116082862A (en) * | 2023-01-09 | 2023-05-09 | 中国矿业大学 | Method for reducing and purifying ash of waste tire pyrolysis carbon black |
| EP4582187A1 (en) * | 2024-01-05 | 2025-07-09 | Orion Engineered Carbons GmbH | Flotation of recovered carbon black |
| EP4582186A1 (en) * | 2024-01-05 | 2025-07-09 | Orion Engineered Carbons GmbH | Gasification and flotation of carbon black |
| EP4582188A1 (en) * | 2024-01-05 | 2025-07-09 | Orion Engineered Carbons GmbH | Gasification of recovered carbon black |
| WO2025146457A1 (en) * | 2024-01-05 | 2025-07-10 | Orion Engineered Carbons Gmbh | Flotation of recovered carbon black |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113563743A (en) * | 2021-07-09 | 2021-10-29 | 中国化学工业桂林工程有限公司 | A kind of catalytic regeneration method of cracking carbon black |
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| EP4582187A1 (en) * | 2024-01-05 | 2025-07-09 | Orion Engineered Carbons GmbH | Flotation of recovered carbon black |
| EP4582186A1 (en) * | 2024-01-05 | 2025-07-09 | Orion Engineered Carbons GmbH | Gasification and flotation of carbon black |
| EP4582188A1 (en) * | 2024-01-05 | 2025-07-09 | Orion Engineered Carbons GmbH | Gasification of recovered carbon black |
| WO2025146457A1 (en) * | 2024-01-05 | 2025-07-10 | Orion Engineered Carbons Gmbh | Flotation of recovered carbon black |
| WO2025146450A1 (en) * | 2024-01-05 | 2025-07-10 | Orion Engineered Carbons Gmbh | Gasification and flotation of carbon black |
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