CN115418119A - Modification method and application of waste tire pyrolytic carbon black - Google Patents
Modification method and application of waste tire pyrolytic carbon black Download PDFInfo
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- 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
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- C09C1/56—Treatment of carbon black ; Purification
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- 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
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention relates to the technical field of carbon black materials, in particular to a modification method and application of waste tire pyrolytic carbon black. Adding dodecylbenzene sulfonic acid, modifying pyrolytic carbon black by an in-situ ball milling method under the action of a ball mill, and preparing the modified pyrolytic carbon black by centrifugal separation and drying in an oven. According to the invention, through modification treatment on the pyrolytic carbon black, the aggregation condition of the pyrolytic carbon black can be improved, re-aggregation of pyrolytic carbon black particles can be effectively prevented, and meanwhile, the pyrolytic carbon black particles are gradually crushed from a submicron level to a nanometer level, a stable dispersion system is formed under the electrostatic repulsion action and the steric hindrance action among the particles, and the dispersion stability of the pyrolytic carbon black is improved. The modified pyrolytic carbon black can partially replace commercial carbon black, has a certain reinforcing effect on natural rubber, and has a relatively wide application prospect.
Description
Technical Field
The invention relates to the technical field of high-value utilization of waste tire pyrolysis products, in particular to a modification method and application of waste tire pyrolysis carbon black
Background
Along with the rapid development of the transportation industry, the demand of tires for vehicles is greatly increased, and the problem that the tire consumption becomes waste tires is increasingly highlighted, so that the environmental risk of recycling the waste tires and the comprehensive utilization of the waste tires as resources are widely concerned. Among various ways of recycling and disposing the waste tires, pyrolysis is a process technology means which is generally recognized to have better resource utilization prospect.
One of the main products of pyrolysis of waste tires is pyrolytic carbon black, which can only be used as an additive for low-value rubber products due to the change of the structural composition and various materials such as commercial zinc oxide and sulfur added in the production process of tires, and the ideal high-value way of pyrolytic carbon black is to reuse the pyrolytic carbon black as a composite material for manufacturing tires.
The reinforcing material of rubber has important practical significance. The strong self-polymerization among carbon black particles makes the carbon black particles difficult to uniformly disperse in a rubber matrix, and further improvement of the performance of the rubber material is limited to a great extent. The modified pyrolytic carbon black is used as a reinforcing material of rubber, and has important practical significance. The dispersibility of the modified carbon black in a rubber matrix is greatly improved, the limitation of the carbon black on enhancing the mechanical property of the rubber is broken through to a certain extent, and other excellent properties are also endowed.
The added surfactant can improve the dispersion effect of the carbon nano material, but the dispersion effect is obviously influenced by the dispersion mode, and if the amount of the added surfactant is only increased without increasing the adsorption amount of the carbon nano material surface, the improvement of the dispersion effect of the material is very limited.
The carbon nano material and the surfactant are subjected to wet ball milling together, amphoteric organic weak acid Dodecyl Benzene Sulfonic Acid (DBSA) with hydrophilic groups and hydrophilic oil groups is added under the action of a mechanical force field provided by ball milling force chemistry, carbon black aggregates and agglomerates are broken, the activated carbon black surface can adsorb DBSA molecules, and the DBSA molecules and the carbon black are coated on the carbon black surface through an intermolecular strong pi-pi conjugate effect. The DBSA molecules realize the stable dispersion of carbon black particles in an aqueous medium through electrostatic repulsion and steric hindrance effect among the particles.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to improve the application value of the waste tire pyrolysis product, especially the pyrolysis carbon black, so as to solve the problems of narrow application range and low economic value of the waste tire pyrolysis carbon black in the prior application technology.
The second purpose of the invention is to provide modified pyrolytic carbon black to improve the performance of the pyrolytic carbon black and solve the technical problem of poor dispersibility of the pyrolytic carbon black in a rubber matrix in the prior art.
The third purpose of the invention is to provide a preparation method of the modified pyrolytic carbon black and to propose the application of the modified pyrolytic carbon black in rubber products.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
dissolving 1 part of dodecyl benzene sulfonic acid in 6.2 parts of deionized water according to mass fraction;
the dodecylbenzene sulfonic acid solution was transferred to a ball mill tank, and then 0.8 part of pyrolytic carbon black was added thereto so that the mass fraction of the pyrolytic carbon black was 10wt%.
In order to realize good nodular graphite effect of the ball mill, the volume of the grinding balls added into the tank is required to be more than 1/3 of the total volume, and the total volume of the grinding balls and materials is less than 3/4 of the volume of the tank
Setting parameters such as rotating speed, ball milling time and the like
And after the ball milling is finished, taking out the ball-milled modified carbon black mixed suspension, centrifuging for 15min at the rotating speed of 5000 revolutions per minute in a centrifuge, and separating out the modified carbon black.
And (3) drying the separated modified carbon black in an oven at 105 ℃ to constant weight.
The invention also provides application of the modified pyrolytic carbon black in preparation of rubber products.
In a particular embodiment of the invention, the modified pyrolytic carbon black is loaded in an amount of 0 to 30phr and the carbon nanotubes are loaded in an amount of not more than 2phr.
Compared with unmodified pyrolytic carbon black, the pyrolytic carbon black of the waste tire modified by the method has better reinforcing property, and the action principle is as follows:
(1) The impact action generated by a strong mechanical force field in the ball milling process enables the pyrolytic carbon black aggregate to be continuously broken to form an active surface, and a large amount of DBSA molecules are adsorbed on the surface of the DBSA molecules through Van der Waals force;
(2) The DBSA molecules adsorbed on the surface of the pyrolytic carbon black have strong hydrophilic sulfonic acid groups and rigid benzene ring structures, and form a strong pi-pi conjugated system with compressed benzene rings on the surface of the pyrolytic carbon black, so that the reaggregation of pyrolytic carbon black particles can be prevented.
With the increase of the ball milling time, submicron-sized pyrolytic carbon black particles are gradually crushed into nanoscale modified carbon black, and a stable dispersion system is formed due to the electrostatic repulsion and steric hindrance between the particles.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method takes pyrolytic carbon black which is one of main products produced by pyrolysis of the waste tires as a raw material, so as to prepare the modified pyrolytic carbon black with good quality, the raw material has wide sources and sufficient supply, the acquisition cost is relatively low, the resource utilization efficiency of the pyrolytic products of the waste tires is improved, and the economic added value of the resource products is increased;
(2) The invention successfully prepares the DBSA coated modified pyrolytic carbon black which can be stably dispersed in the aqueous solution by using an in-situ ball milling modification method, the production process is carried out in a liquid phase, no dust is blown, the pollution is small, and the obtained product has the characteristic of environmental friendliness;
(3) The modified pyrolytic carbon black obtained by the invention has stable quality, good performance and certain reinforcing effect, can partially replace commercial carbon black to be used for manufacturing rubber products, and has wide application prospect.
Drawings
FIG. 1 is a flow chart illustrating the preparation of a modified pyrolytic carbon black of the present invention;
FIG. 2 is a surface topography of a pyrolytic carbon black before modification;
FIG. 3 shows the surface morphology of the modified pyrolytic carbon black.
FIG. 4 is a mechanical property index of the present invention;
in the figure, (a) tensile strength; (b) elongation at break; (c) a constant extension force of 100%; (d) 100% stress at definite elongation; (e) a constant extension force of 300%; (f) 300% stress at definite elongation; (g) hardness.
Detailed Description
While the technical solutions of the present invention will be described clearly and completely with reference to the specific embodiments, those skilled in the art will understand that the following described examples are some, but not all, examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The waste tire pyrolytic carbon black subjected to modification treatment by the method has good dispersion performance and good interface compatibility with organic polymer materials represented by natural rubber.
Compared with unmodified pyrolytic carbon black, the pyrolytic carbon black of the waste tire modified by the method has better reinforcing performance, and can partially replace the existing commercial carbon black.
As shown in fig. 1, in the embodiment of the present invention, the modified pyrolytic carbon black is mainly obtained by a ball milling tank added with a dodecylbenzene sulfonic acid solution, and is treated by a ball mill in-situ ball milling method. The main components are as follows by weight:
0.8 part of pyrolytic carbon black powder, 1 part of dodecylbenzene sulfonic acid and 6.2 parts of deionized water.
In a specific embodiment of the invention, the pyrolytic carbon black powder is waste tire pyrolytic carbon black powder.
Further, the waste tires are divided according to types, including but not limited to any one or more of waste all-steel tires, waste semi-steel tires and waste bias tires;
further, the junked tires are classified by source, including but not limited to any one or more of truck junked tires, passenger car junked tires, bicycle junked tires, motorcycle junked tires;
further, the source of scrap tires does not include aircraft scrap tires.
In practical operation, the waste tire pyrolytic carbon black powder is prepared by a micro-negative pressure rotary kiln pyrolytic reactor.
Further, scrap tire pyrolytic carbon black powder prepared by a conventional method can also be used as a raw material in the practice of the present invention.
In a specific embodiment of the present invention, the pyrolytic carbon black powder is obtained by pyrolysis of scrap tires from which steel wires have been previously removed.
In a specific embodiment of the present invention, the pyrolytic carbon black powder is obtained by a 120-mesh sieve treatment in advance.
In a particular embodiment of the invention, the temperature conditions are room temperature, preferably 25 ℃.
In a specific embodiment of the present invention, the rotation speed of the ball milling process is 5000rpm.
In a specific embodiment of the present invention, the temperature of the forced air drying is 150 ℃ and the drying time is 30 minutes.
The invention also provides application of the modified pyrolytic carbon black in preparation of rubber products.
In a particular embodiment of the invention, the rubber article further comprises commercial carbon black, stearic acid, zinc oxide, accelerators and vulcanizing agents.
The commercial carbon black is a commercial tire rubber reinforcing agent, preferably commercial high-abrasion-resistance carbon black N330, and meets the GB 3778-2003 standard.
The accelerator is an accelerator DM, and the vulcanizing agent is sulfur.
Examples
This example provides a method for preparing a modified pyrolytic carbon black, comprising the steps of:
(1) And (3) screening the waste tire pyrolytic carbon black through a 120-mesh screen to obtain the raw material pyrolytic carbon black powder used in the examples for later use.
(2) Preparation of dodecyl benzene sulfonic acid solution: dissolving dodecyl benzene sulfonic acid with the purity of 90% in deionized water, wherein the mass ratio of a solute to a solvent is 1: preparing a dodecyl benzene sulfonic acid solution according to the proportion of 6.2 for later use.
(3) And (3) weighing 90 parts by weight of the dodecyl benzene sulfonic acid solution prepared in the step (2), transferring the solution to a ball milling tank, and adding 10 parts of the pyrolytic carbon black powder prepared in the step (1). And (3) adding grinding balls into the ball milling tank, wherein the volume of the magic ball is more than 1/3 of the total volume, and the total volume of the grinding balls and the materials is less than 3/4 of the volume of the tank. After canning, the ball mill can is placed into a ball mill puller sleeve and symmetrically installed, after installation, the V-shaped bolt is screwed down by using the two stress application sleeves, and then the locking nut is screwed down to prevent the ball mill can from loosening during ball milling. After the ball milling tank is installed, the protective cover is covered, parameters such as rotating speed, ball milling time and the like are set, and the ball milling instrument is operated after the safety switch is turned on.
And after the ball milling is finished, taking out the ball-milled modified carbon black mixed suspension, centrifuging for 15 minutes in a centrifuge at 5000rpm, separating out the modified pyrolytic carbon black, drying in an oven at 105 ℃ to constant weight, and storing in a dryer.
The surface topography of the pyrolytic carbon black before modification is shown in FIG. 2:
FIG. 3 shows the surface morphology of the modified pyrolytic carbon black as shown in the figure:
to illustrate the difference in reinforcing properties of different modified pyrolytic carbon blacks at different addition ratios, examples 1-6 were prepared according to different addition ratios and formulations of modified pyrolytic carbon blacks, respectively, and the formulations of the compounds are shown in the following table
TABLE 1 preparation formulation of modified pyrolytic carbon Black/commercial carbon Black N330/Natural rubber composites
The preparation of the modified pyrolytic carbon black/commercial carbon black N330/natural rubber composite material in the above example is carried out according to the national standard GB/T3780.18-2017 identification method of carbon black part 18 in Natural Rubber (NR), and the modified pyrolytic carbon black/commercial carbon black/natural rubber composite material is prepared by a mechanical blending method, and mainly comprises the following steps:
after the bin of the internal mixer, the two rollers of the open mill and the operating table are cleaned, a small amount of natural rubber is used for washing the rollers of the internal mixer until no dust is left on the rollers, then the rollers are put into the internal mixer, the internal mixer is operated for about 3 minutes to increase the initial temperature, and then the natural rubber is taken out. The mixing is divided into two steps, and the two steps are respectively carried out in an internal mixer and an open mill. When the process is carried out in an internal mixer, the initial temperature of a bin is controlled to be about 70 ℃, and the rotating speed of a rotor is 50r/min. After the composite material is prepared, the rubber is placed for at least 24 hours and then is vulcanized.
The main steps for preparing vulcanized rubber by vulcanization treatment are as follows:
and testing the vulcanization characteristic of the rubber compound by using a rotor-free vulcanizing instrument, and preparing a vulcanization sample by using a flat vulcanizing instrument according to the positive vulcanization time of the process.
When the rubber sheet is vulcanized on a flat vulcanizing machine, the temperature is controlled at 150 ℃ for 30min, and the vulcanized rubber sheet forms a uniform sheet with the thickness of about 2mm in a mould.
To illustrate the differences in the crosslinking degree of the composite systems of the vulcanizates at different ratios of the modified pyrolytic carbon black, the vulcanization characteristic curves of examples 1-6 were tested, respectively, and the data obtained are shown in the following table:
TABLE 2 modified pyrolytic carbon Black/commercial carbon Black N330/Natural rubber composites vulcanization parameters
In order to compare and illustrate the difference of the mechanical properties of vulcanized rubber under different addition proportions of the modified pyrolytic carbon black,
examples 1 to 6 were tested for mechanical properties including tensile strength, elongation at break, tensile strength at set elongation, stress at set elongation, and the like. The data obtained are shown in FIG. 4:
in the figure: (a) tensile strength; (b) elongation at break; (c) a constant extension force of 100%; (d) 100% stress at definite elongation; (e) a constant extension force of 300%; (f) 300% stress at definite elongation; (g) Hardness of
FIG. 1 mechanical Properties of modified pyrolytic carbon Black/commercial carbon Black N330/Natural rubber composite as a function of the amount of modified pyrolytic carbon Black added
The test results show that the modified pyrolytic carbon black prepared by the invention has good reinforcing performance, can be used together with commercial carbon black N330 in a formula, can partially replace commercial carbon black, enhances the dispersibility of the pyrolytic carbon black in a rubber matrix, and improves the application value of the pyrolytic carbon black. The modified pyrolytic carbon black prepared by the method has wide prospect when being used as a reinforcing material in the field of rubber.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. The modified pyrolytic carbon black is characterized in that dodecyl benzene sulfonic acid solution is mainly added, and the modified pyrolytic carbon black is prepared by in-situ ball milling treatment under the action of a ball mill, centrifugal separation and drying in an oven.
2. The modified pyrolytic carbon black of claim 1, wherein the average particle size of the modified pyrolytic carbon black is 350-450nm, and the S and Zn contents in the modified pyrolytic carbon black are reduced by 84% and 65%, respectively;
preferably, the pyrolytic carbon black powder is carbon black powder obtained by pyrolyzing waste tires in a micro-negative pressure rotary kiln.
3. The modified pyrolytic carbon black according to claim 1, wherein the preparation of the dodecylbenzene sulfonic acid solution comprises: placing dodecyl benzene sulfonic acid in deionized water, and obtaining the dodecyl benzene sulfonic acid solution at 25 ℃;
preferably, the mass ratio of the dodecylbenzene sulfonic acid to the deionized water is 1:6.2.
4. the modified pyrolytic carbon black of claim 1, wherein the modified pyrolytic carbon black is ball-milled and modified by adding pyrolytic carbon black to a dodecylbenzene sulfonic acid solution;
preferably, the mass fraction of the pyrolytic carbon black is 10wt%;
preferably, the volume of the grinding ball in the tank is more than 1/3 of the total volume, and the total volume of the grinding ball and the material is less than 3/4 of the volume of the tank.
5. The modified pyrolytic carbon black of claim 1, wherein the modified pyrolytic carbon black powder is subjected to centrifugal separation and drying at constant temperature;
preferably, the centrifuge speed is 5000 rpm;
preferably, the centrifugation time is 15 minutes;
preferably, the oven temperature is 105 ℃.
6. The method of any one of claims 1-4, wherein the aggregates of the particles of the modified pyrolytic carbon black are ellipsoidal and have a size of 250nm x 150nm.
7. Use of the modified pyrolytic carbon black of any one of claims 1-6 in the preparation of a rubber article;
preferably, the modified pyrolytic carbon black is loaded in an amount of 0 to 30phr;
preferably, the modified pyrolytic carbon black-filled rubber incorporates carbon nanotubes.
8. Use of the modified pyrolytic carbon black of claim 7 in the preparation of rubber articles, wherein the fillable carbon nanotubes promote the formation of a crosslinked network;
preferably, the loading of carbon nanotubes is not greater than 2phr.
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| JPH0680917A (en) * | 1992-08-31 | 1994-03-22 | Pentel Kk | Ink for making thermal stencil sheet |
| JP2006160944A (en) * | 2004-12-09 | 2006-06-22 | Yokohama Rubber Co Ltd:The | Production of master batch of natural rubber/carbon black |
| CN106084336A (en) * | 2016-07-25 | 2016-11-09 | 浙江传化合成材料有限公司 | A kind of wet method carbonblack master batch and its preparation method and application |
| CN111499938A (en) * | 2020-04-15 | 2020-08-07 | 青岛科技大学 | Continuous mixing method and device for carbon black formula rubber |
| CN111662576A (en) * | 2019-03-07 | 2020-09-15 | 青岛四维化工有限公司 | Preparation method of quasi-in-situ modified pyrolytic carbon black |
-
2022
- 2022-07-06 CN CN202210789271.4A patent/CN115418119A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0680917A (en) * | 1992-08-31 | 1994-03-22 | Pentel Kk | Ink for making thermal stencil sheet |
| JP2006160944A (en) * | 2004-12-09 | 2006-06-22 | Yokohama Rubber Co Ltd:The | Production of master batch of natural rubber/carbon black |
| CN106084336A (en) * | 2016-07-25 | 2016-11-09 | 浙江传化合成材料有限公司 | A kind of wet method carbonblack master batch and its preparation method and application |
| CN111662576A (en) * | 2019-03-07 | 2020-09-15 | 青岛四维化工有限公司 | Preparation method of quasi-in-situ modified pyrolytic carbon black |
| CN111499938A (en) * | 2020-04-15 | 2020-08-07 | 青岛科技大学 | Continuous mixing method and device for carbon black formula rubber |
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