CN114736539A - Scrap old tire carbon black deep treatment process and granulation method thereof - Google Patents
Scrap old tire carbon black deep treatment process and granulation method thereof Download PDFInfo
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- CN114736539A CN114736539A CN202210517175.4A CN202210517175A CN114736539A CN 114736539 A CN114736539 A CN 114736539A CN 202210517175 A CN202210517175 A CN 202210517175A CN 114736539 A CN114736539 A CN 114736539A
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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
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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
- C09C1/56—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
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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
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/58—Agglomerating, pelleting, or the like by wet methods
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the field of resource recycling, in particular to a scrap old tire carbon black deep treatment process and a granulation method thereof, which comprises the steps of (1) pretreatment; (2) activating; (3) and (6) granulating. The invention enhances the compatibility with rubber by modifying and granulating the surface of the carbon black, achieves the performance index of the industrial carbon black, improves the added value of the pyrolytic carbon black, greatly increases the economic benefit of enterprises, and adopts the low-concentration perchloric acid in the activation process, so that the carbon black is not consumed, harmful gas is not generated, and the invention is safe and reliable.
Description
Technical Field
The invention relates to the field of resource recycling, in particular to a scrap old tire carbon black deep treatment process and a granulation method thereof.
Background
With the increasing use amount of automobiles, the use amount of tires is more and more, which causes a great amount of accumulated waste tires, resulting in serious black pollution, and the recycling of the waste tires is a major issue in the world today. The recycling of waste tires in China in the future is expected to be a sunrise industry, and the common mode of recycling the waste tires mainly comprises the following steps: retreading tires, thermal cracking, producing rubber powder and the like. Because the carbon content of the waste tires is high, researchers mostly consider researching and preparing activated carbon and carbon black products, and the common preparation of the carbon black products from the waste tires is to carry out thermal cracking treatment on the waste tires, and then take residues obtained after the thermal cracking treatment as the carbon black products; however, such carbon black products have high environmental pollution, high ash content, poor dispersibility and poor compatibility with rubber.
Chinese patent CN 109504134A discloses a process for producing carbon black from waste tires, which comprises the steps of crushing waste tires without iron wires, activating and catalytically cracking the waste tires to obtain carbon black, drying the carbon black, adding an alkaline agent, neutralizing the carbon black, drying the carbon black, adding concentrated sulfuric acid for oxidation, adding isocyanate for bonding with hydroxyl on the surface of the carbon black, mixing the carbon black and water in a pre-mixer, granulating the mixture, and drying the mixture in a drying kiln to obtain a finished product. The patent enhances the compatibility with rubber by crushing, classifying, screening, surface modifying and granulating the primary carbon black. However, the carbon black is oxidized by adopting concentrated sulfuric acid, on one hand, the concentrated sulfuric acid is a strong corrosive reagent, and the danger in the use process is great; on the other hand, concentrated sulfuric acid has strong oxidizing property, and can react with carbon black to consume part of the carbon black, and particularly the reaction can generate sulfur dioxide gas (C + 2H)2SO4(concentrated) → CO2↑+2SO2↑+2H2O), causing environmental pollution. It has been proposed to use nitric acid instead of concentrated sulfuric acid, however, through a lot of experiments, the inventor found that the oxidation effect required for preparing carbon black cannot be achieved when the concentration of nitric acid is low, the nitric acid also reacts with carbon black to consume part of carbon black, and nitrogen oxide gas (C +4 HNO) is generated to harm the environment3(concentrated) → CO2↑+4NO2↑+2H2O). Other oxidizing acids, such as hydrochloric acid, are too volatile to be used.
Therefore, how to optimize the process of preparing carbon black from waste tires becomes a key research project for waste tire treatment and recycling application.
Disclosure of Invention
The invention aims to provide a scrap old tire carbon black deep treatment process and a granulation method thereof, which can solve the problems of strong danger, large carbon black loss, harmful gas generation and the like in the carbon black activation process.
In order to achieve the purpose, the invention adopts the technical scheme that: a scrap old tire carbon black deep treatment process and a granulation method thereof comprise the following steps:
(1) pretreatment: the method comprises the following steps of (1) carrying out pyrolysis and carbonization process treatment on waste tires to obtain carbon slag, carrying out magnetic separation and iron removal, and grinding to a particle size meeting the standard of industrial carbon black to obtain a carbon black precursor;
(2) and (3) activation: mixing carbon black precursor with 1.5-2.5mol/L HClO4Mixing the water solution in a ratio of 1g/7-15ml, reacting for 0.5-1h, filtering to obtain acid-washed carbon black, soaking the acid-washed carbon black in an organic solvent, and drying to obtain a carbon black activated material;
(3) and (3) granulation: and mixing the carbon black activating material with the carbon nano tube, the tryptophan and the lactose aqueous solution, uniformly stirring, granulating, and drying to obtain the granulated carbon black.
The mechanism of the invention is as follows: tyre cracking due to the different processes and corresponding tyre sources, the ash content is higher than that of the commercial carbon black, generally ranging from 10 wt.% to 25 wt.%, and the ash covers the active sites of the carbon black and prevents the direct contact of the surface of the carbon black with rubber molecules, said use of HClO4After cleaning, the ash content and the oil content on the surface of the carbon black are reduced, micropores of the carbon black are increased, and the covered holes of the carbon black are reopened because of HClO4The strong oxidizing acid oxidizes the organic matters on the surface of the carbon black, so that new micropores are formed, and the adsorption capacity of the carbon black is improved; and the used perchloric acid has low concentration, greatly reduced danger, no volatilization, no generation of harmful gas and environmental friendliness.
The pyrolysis oil covers the surface of the carbon black, so that the specific surface area of the carbon black is reduced, the pyrolysis oil can shield active points on the surface of the carbon black and hinder the interaction between the carbon black and rubber molecular chains, the stress at definite elongation of the rubber is reduced, the rubber is soaked and extracted by an organic solvent, and the specific surface area is further improved after the oil is extracted and removed; on the other hand, with HClO4After acid washing, a small amount of organic matters are generated and attached to carbon black, so that the acid washing effect is influenced, and the treatment of an organic solvent just makes up for the adoption of HClO4The insufficiency of acid washing, the loose arrangement among carbon black aggregates and the change of the gaps among the aggregatesThe content of micropores and mesopores on the surface of the carbon black is increased, and the adsorbability of the carbon black is improved.
In addition, the surface energy of the carbon black is higher than that of rubber, agglomeration is easy to occur, common high-molecular saturated lipids are limited in molecular weight, and the agglomeration phenomenon is difficult to completely solve due to the dispersing effect.
The lactose has high cohesiveness and chelatability, and can highly fuse, aggregate and granulate carbon black, carbon nanotubes and tryptophan, thereby improving the granulation effect.
In the step (1), the particle size of the carbon black precursor is 300-400 meshes. The carbon black particle size can be adjusted according to the requirements of users.
In the step (2), carbon black precursor and HClO4And (3) mixing the aqueous solutions, mechanically stirring for 0.5-1 hour in a constant-temperature water bath at 50 ℃, cooling, performing suction filtration, washing with water to pH 7-9, and continuing suction filtration to obtain the acid-washed carbon black. The organic solvent is one or more of ethanol, benzene, toluene, acetone, acetonitrile, ethanolamine, formamide and the like. Mixing the acid-washed carbon black and an organic solvent according to the proportion of 1g/5-20ml, mechanically stirring for 30-45 minutes, heating and extracting until an extract is colorless, completely removing the organic solvent, and drying in a drying oven at 105 ℃ to constant weight to obtain the carbon black activated material.
In the step (3), the carbon nano tube, the tryptophan and the lactose aqueous solution are uniformly mixed according to the mass ratio of (0.2-8) to (0.1-10) to (40-100) to prepare a granulation liquid, and then the carbon black activated material and the granulation liquid are mixed for granulation. The mass concentration of the lactose aqueous solution is 3-15%, and the lactose aqueous solution is added for 2-3 times to improve the mixing effect. The carbon black activating material and the granulating liquid are mixed according to the mass ratio of (5-8) to 4 for granulation, and the granularity of the granulated carbon black is (3 +/-0.5) mm.
The invention enhances the compatibility with rubber by modifying and granulating the surface of the carbon black, achieves the performance index of the industrial carbon black, improves the added value of the pyrolytic carbon black, greatly increases the economic benefit of enterprises, and adopts the low-concentration perchloric acid in the activation process, so that the carbon black is not consumed, harmful gas is not generated, and the invention is safe and reliable.
Detailed Description
The technical solution of the present invention is further described below with reference to examples and test data.
Preparing a carbon black precursor: after the waste tires are treated by a cracking carbonization process, carbon slag discharged from a thermal cracking reactor is magnetically deironing by a magnetic iron remover of a pretreatment unit, so that iron filings of steel wires are removed to form crude carbon black and the crude carbon black is recycled by a storage bin; the crude carbon black was subjected to ultrafine grinding by a carbon black powder pulverizer to obtain a carbon black precursor having a particle size of 300 mesh, which was used in the following examples and comparative examples.
Example 1
And (3) activation: preparing 2mol/L HClO42L, placing the carbon black precursor and acid liquor into an activation container according to the proportion of 1g/10ml, mechanically stirring for 1 hour at the constant temperature of 50 ℃, cooling, carrying out suction filtration and water washing until the pH value is 7, continuing suction filtration, and collecting to obtain acid-washed carbon black; placing acid-washed carbon black and an organic solvent into a beaker according to the proportion of 1g/5ml, mechanically stirring the mixture of the organic solvent ethanol, benzene, toluene, acetone, acetonitrile, ethanolamine and formamide for 45 minutes, heating and extracting until the extract is colorless, removing the organic solvent, and drying in a drying oven at 105 ℃ until the weight is constant to obtain the carbon black activated material.
And (3) granulation: mixing a carbon nano tube, tryptophan and a 10% lactose aqueous solution according to the mass ratio of 1:1.2:50, stirring for 1h in a stirring kettle at the normal pressure and 60 ℃, adding the lactose aqueous solution for 3 times, uniformly stirring to obtain a granulating liquid, conveying a carbon black activating material and the granulating liquid according to the mass ratio of 6:4 to a granulator through a pipeline, stirring for 40 minutes, granulating wet carbon black particles, and conveying the carbon black particles to a drying roller through a discharge pipe for drying to obtain the granulated carbon black with the particle size of about 3 mm.
Examples 2-1 and 2-2
Activation and granulation were carried out in the same manner as in example 1, except that the acid-washed carbon black and the acid solution were used in a ratio of 1g/15ml and 1g/7ml, respectively.
Examples 3-1 and 3-2
The activation and granulation were carried out by the method of example 1, wherein the ratios of the acid-washed carbon black to the organic solvent were 1g/10ml and 1g/15ml, respectively, and the other conditions and data were the same.
Examples 4-1 and 4-2
The activation and granulation were carried out by the method of example 1, wherein the concentrations of the lactose aqueous solution were 5% and 15%, respectively, and the other conditions and data were the same.
Comparative example
The carbon black precursor was directly pelletized according to the pelletizing procedure reported in example 1 to obtain pelletized carbon black.
The pelletized carbon blacks obtained in the above examples and comparative examples were tested for various performance parameters and are included in the following table:
the invention has good carbon black surface modification and granulation effects, and the comparison of the research data in the table shows that compared with original non-activated granulated carbon black, the properties of the granulated carbon black after activation and regeneration are obviously greatly improved, and the iodine absorption value of 89.4g/kg can prove that the adsorption capacity of the carbon black is greatly improved by observing the research data of the iodine absorption value and the adsorption specific surface area of the carbon black; the study data from 45 μm sieve residue and pour density were: the 45 μm screen residue was 473mg/kg, less than 500mg/kg, and it was found that the present invention has a high granulation rate of carbon black with a pour density of 458kg/m3The volume of the carbon black in unit mass is obviously reduced, and the granulation quality is obviously improved; from 3The research data of the stress at definite elongation of 00 percent can prove that the invention enhances the compatibility of the granulated carbon black and the rubber, enhances the activity and enlarges the stress at definite elongation, reaches the service performance index of the industrial carbon black, improves the use field of the carbon black, increases the economic benefit of the carbon black, realizes the recycling and comprehensive utilization of resources and actively responds to the policy of 'carbon emission reduction and carbon peak reaching' in the fourteen-five planning of China.
Claims (10)
1. A scrap old tire carbon black deep treatment process and a granulation method thereof comprise the following steps:
(1) pretreatment: the method comprises the following steps of (1) carrying out pyrolysis and carbonization process treatment on waste tires to obtain carbon slag, carrying out magnetic separation and iron removal, and grinding to a particle size meeting the standard of industrial carbon black to obtain a carbon black precursor;
(2) activation: mixing carbon black precursor with 1.5-2.5mol/L HClO4Mixing the water solution in a ratio of 1g/7-15ml, reacting for 0.5-1h, filtering to obtain acid-washed carbon black, soaking the acid-washed carbon black in an organic solvent, and drying to obtain a carbon black activated material;
(3) and (3) granulation: and mixing the carbon black activating material with the carbon nano tube, the tryptophan and the lactose aqueous solution, uniformly stirring, granulating, and drying to obtain the granulated carbon black.
2. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 1 are characterized in that: in the step (1), the particle size of the carbon black precursor is 300-400 meshes.
3. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 1 are characterized in that: in the step (2), carbon black precursor and HClO4And (3) mixing the aqueous solutions, mechanically stirring in a constant-temperature water bath at 50 ℃ for 0.5-1 hour, cooling, performing suction filtration, washing with water to pH 7-9, and continuing suction filtration to obtain the acid-washed carbon black.
4. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 1 are characterized in that: in the step (2), the organic solvent is one or more of ethanol, benzene, toluene, acetone, acetonitrile, ethanolamine, formamide and the like.
5. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 1 are characterized in that: in the step (2), acid-washing carbon black and an organic solvent are mixed according to the proportion of 1g/5-20ml, the mixture is mechanically stirred for 30-45 minutes, the mixture is heated and extracted until the extract is colorless, the organic solvent is thoroughly removed, and the mixture is placed in a drying oven at 105 ℃ and dried to constant weight, so that the carbon black activated material is obtained.
6. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 1 are characterized in that: in the step (3), the carbon nano tube, the tryptophan and the lactose aqueous solution are uniformly mixed according to the mass ratio of (0.2-8) to (0.1-10) to (40-100) to prepare a granulation liquid, and then the carbon black activating material and the granulation liquid are mixed for granulation.
7. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 6 are characterized in that: the mass concentration of the lactose aqueous solution is 3-15%.
8. The carbon black deep treatment process and the granulation method thereof for scrap old tires according to claim 6 are characterized in that: lactose solution is added in 2-3 times.
9. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 6 are characterized in that: and mixing the carbon black activating material and the granulating liquid according to the mass ratio of (5-8) to (4) for granulating.
10. The carbon black deep treatment process and the granulation method for the used scrap tire according to claim 1 are characterized in that: in the step (3), the particle size of the pelletized carbon black is (3. + -. 0.5) mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116640467A (en) * | 2023-05-26 | 2023-08-25 | 安徽固瑞特新材料科技有限公司 | Environment-friendly activation production process for recycling carbon black from high-quality waste tires |
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