CN117986898A - Modified cracking carbon black and preparation method thereof - Google Patents
Modified cracking carbon black and preparation method thereof Download PDFInfo
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- 238000005336 cracking Methods 0.000 title claims abstract description 153
- 239000006229 carbon black Substances 0.000 title claims abstract description 125
- 238000002360 preparation method Methods 0.000 title abstract description 38
- 238000000227 grinding Methods 0.000 claims abstract description 108
- 229920005989 resin Polymers 0.000 claims abstract description 60
- 239000011347 resin Substances 0.000 claims abstract description 60
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 238000012986 modification Methods 0.000 claims abstract description 38
- 230000004048 modification Effects 0.000 claims abstract description 38
- 150000002148 esters Chemical class 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 42
- 238000007885 magnetic separation Methods 0.000 claims description 30
- 235000021355 Stearic acid Nutrition 0.000 claims description 29
- 239000003963 antioxidant agent Substances 0.000 claims description 29
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 29
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 29
- 239000008117 stearic acid Substances 0.000 claims description 29
- 230000003078 antioxidant effect Effects 0.000 claims description 27
- -1 polyene ester Chemical class 0.000 claims description 25
- 239000010920 waste tyre Substances 0.000 claims description 24
- 238000003763 carbonization Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 16
- 239000003292 glue Substances 0.000 claims description 14
- 239000002390 adhesive tape Substances 0.000 claims description 6
- 229920001225 polyester resin Polymers 0.000 claims description 6
- 239000004645 polyester resin Substances 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 238000005498 polishing Methods 0.000 abstract 2
- 235000019241 carbon black Nutrition 0.000 description 105
- 238000002156 mixing Methods 0.000 description 72
- 239000002994 raw material Substances 0.000 description 15
- 229910000831 Steel Inorganic materials 0.000 description 13
- 239000002245 particle Substances 0.000 description 13
- 239000010959 steel Substances 0.000 description 13
- 238000010000 carbonizing Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 230000010287 polarization Effects 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 230000002934 lysing effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
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Abstract
The invention discloses modified cracking carbon black and a preparation method thereof, and belongs to the technical field of cracking carbon black production. The method includes a polishing modification treatment step, the polishing modification treatment step further including: premixing the cracked carbon black and the polyenoic ester resin to prepare a mixture A, grinding the mixture A and other auxiliary agents, wherein the grinding speed is any value of 30-50 rpm, and the induced air speed is any value of 28-36 rpm. The invention is applied to the production of the cracking carbon black, solves the further application problem that the cracking carbon black product obtained by the prior cracking technology cannot be well applied due to low performance, can effectively improve the surface activity of the cracking carbon black, and the obtained modified cracking carbon black has the characteristics of reinforcing property and excellent wear resistance.
Description
Technical Field
The invention belongs to the technical field of production of cracked carbon black, and particularly relates to a blending grinding modified cracked carbon black and a preparation method thereof.
Background
With the rapid development of the economic society in China, the maintenance amount of vehicles such as household vehicles, passenger and cargo transportation vehicles, engineering vehicles and the like is rapidly increased, the rapidly developed automobile market also causes the rapid increase of the number of waste tires, and if the waste tires are improperly treated, the environment is seriously polluted. Therefore, how to properly treat junked tires becomes an important global social responsibility problem. At present, the comprehensive utilization of waste tires is focused on all countries in the world, and the methods for processing the waste tires at home and abroad mainly comprise tire retreading, reclaimed rubber production or reclaimed rubber powder production and thermal cracking. The waste tires are prepared into products such as cracked carbon black, cracked oil, cracked gas, steel wires and the like through crushing, impurity removal and high-temperature cracking by the thermal cracking method, so that the waste tires are thoroughly recycled.
However, the traditional cracking technology still has the defects of high energy consumption, high cost, low performance of the cracked carbon black product and the like. Therefore, how to carry out modification treatment on the cracking carbon black and provide a preparation method of the modified cracking carbon black which has simple preparation process, lower cost and ideal carbon black quality.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to solve the technical problem that the cracking carbon black product obtained by the prior cracking technology cannot be well applied due to low performance, and provides the modified cracking carbon black with the characteristics of effective improvement of the surface activity of the cracking carbon black, excellent reinforcement and wear resistance and the preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
In one aspect, the present invention provides a method for preparing a modified cracked carbon black, comprising a grinding modification treatment step, the grinding modification treatment step further comprising: premixing the cracking carbon black and the polyenoic ester resin to prepare a mixture A, and grinding the mixture A and other auxiliary agents at any value of 30-50 r/s.
Preferably, the polyester resin is selected from LSR-395 resins.
Preferably, the grinding modification treatment step further includes: pushing and grinding the mixture A and other auxiliary agent feed, and sending the ground mixture A and other auxiliary agent feed to a granulating process for granulating by induced air; the feeding frequency is any value of 3-10 Hz; the induced draft rotational speed is any value of 28-36 revolutions per second.
Preferably, the other auxiliary agents include stearic acid and antioxidants.
Preferably, the cracking carbon residue is 100 parts by weight, the stearic acid is any one of 1-5 parts by weight, the antioxidant is any one of 0.2-5 parts by weight, and the polyene ester resin is any one of 1-8 parts by weight.
Preferably, the pre-mixing stirring temperature of the pre-mixing of the cracking carbon black and the polyester resin to obtain the mixture A is any value of 100-120 ℃ and the stirring time is 0.5h.
Preferably, the method further comprises a crushing treatment step, a magnetic separation treatment step and a cracking carbonization treatment step before the grinding modification treatment step.
Preferably, the crushing treatment step includes: firstly, crushing the waste tires in a first section to obtain adhesive tapes, and then crushing the adhesive tapes in a second section to obtain adhesive blocks; the device used for the first-stage crushing treatment is a strip crusher, and the device used for the second-stage crushing treatment is a granular crusher; the grain diameter of the rubber block is less than or equal to 35mm.
Preferably, the step of cracking and carbonizing includes: and (3) conveying the glue blocks treated by the magnetic separation treatment step into a cracking device, and carrying out cracking carbonization treatment at 380-480 ℃ to obtain the cracking carbon residue.
The invention also provides modified cracked carbon black, which is prepared by the preparation method of the modified cracked carbon black in any one of the technical schemes.
Compared with the prior art, the invention has the beneficial effects that:
The invention provides a preparation method of modified cracked carbon black, wherein the polyene ester resin is taken as a polarized resin material, when the cracked carbon black is modified, based on the polarization characteristic of the polyene ester resin, the structure of a carbon black particle aggregate is destroyed by mechanical shearing force during grinding, the variety and the number of surface groups are changed, the surface activity and the polarity are increased, the reagglomeration trend of the carbon black is reduced, the polyene ester resin is grafted to the surface of the cracked carbon black particle, and the cracked carbon black is endowed with good polarization performance, so that the compatibility with various raw materials and auxiliary materials of rubber is good, thereby obtaining a cracked carbon black product with excellent performances, solving the further application problem that the cracked carbon black product obtained by the prior cracking technology cannot be well applied due to low performance, and expanding the application range of the blended superfine grinding modified cracked carbon black in high-performance tires.
Detailed Description
The technical scheme in the specific embodiment of the invention will be fully described in detail. It is apparent that the described embodiments are only some specific implementations, but not all implementations, of the general technical solution of the present invention. All other embodiments, which are obtained by those skilled in the art based on the general inventive concept, fall within the scope of the present invention.
In one aspect, the present invention provides a method for preparing a modified cracked carbon black, comprising a grinding modification treatment step, the grinding modification treatment step further comprising: premixing the cracking carbon black and the polyenoic ester resin to prepare a mixture A, and grinding the mixture A and other auxiliary agents at any value of 30-50 r/s. In a preferred embodiment, the polyester resin is selected from LSR-395 resins. When the polyolefin ester resin is used as a polarized resin material to modify the cracked carbon black, the structure of the carbon black particle aggregates is damaged by the action of mechanical shearing force during grinding, the types and the number of surface groups are changed, the surface activity and the polarity are increased, the reagglomeration trend of the carbon black is reduced, the polyolefin ester resin is grafted to the surface of the cracked carbon black particles, the cracked carbon black is endowed with good polarization performance, the compatibility with various raw materials and auxiliary materials of rubber is good, the surface activity of the cracked carbon black is effectively improved, the dispersibility of the cracked carbon black in the rubber is improved, and thus the modified cracked carbon black product with excellent performances such as reinforcing property, wear resistance and the like is obtained, the further application problem that the cracked carbon black product obtained by the existing cracking technology cannot be well due to low performance is solved, and the application range of the modified cracked carbon black in a high-performance tire is expanded.
In the preparation method, the grinding rotating speed is specifically limited, and the reason is that the grinding rotating speed determines the shearing force of raw materials during grinding, and the method controls the shearing force, so that the cracking carbon black is grafted with the polyene ester resin through sufficient mechanical shearing, meanwhile, the particle size of the cracking carbon black after grinding is uniform, the application requirements of high-performance tires and the like are met, and when the mixture of the cracking carbon black and the polyene ester resin is ground during feeding, all the mixture is fully ground through scientific uniform feeding, so that the polyene ester resin is fully grafted on cracking carbon black molecules.
The technical scheme of the invention further limits the feeding sequence, because the cracked carbon black and the polyenoic ester resin are firstly mixed and stirred in a mixing tank, which is beneficial to the compatibility of the polarization characteristic of the polyenoic ester resin and the rubber interface, and the silicon oxygen group in the cracked carbon black and the polyenoic ester resin need to react under a certain temperature condition and time to modify the cracked carbon black. In a preferred embodiment, the pre-mixing stirring temperature of the pre-mixing of the cracked carbon black and the polyester resin to produce mixture A is any one of 100-120 ℃ and the stirring time is 0.5h. In the temperature and time, the reaction between the silica groups in the cracked carbon black and the polyester resin can be ensured, and the modification of the cracked carbon black is realized.
The preparation method can solve the technical problems of high energy consumption, high cost, low performance of the cracked carbon black product and the like in the prior art, has the characteristics of simple preparation process, controllable cost, excellent performances of the carbon black and the like, and realizes the recycling of waste tire resources. The grinding particle size of the modified cracking carbon black prepared by the method is controlled to be 5-8 mu m, wherein the particle size distribution is obtained by testing the D90 particle size value by a laser particle size analyzer.
In a preferred embodiment, the grinding modification treatment step further comprises: pushing and grinding the mixture A and other auxiliary agent feed, and sending the ground mixture A and other auxiliary agent feed to a granulating process for granulating by induced air; the feeding frequency is any value of 3-10Hz, and the induced draft rotating speed is any value of 28-36 revolutions per second. According to the technical scheme, the feeding frequency is limited, so that the limitation of the feeding frequency is realized, and the uniform feeding is ensured. It will be appreciated that the feed frequency may also be any point value within 4Hz, 5Hz, 6Hz, 7Hz, 8Hz, 9Hz and ranges thereof, and the induced draft speed may also be any point value within 30 revolutions per second, 32 revolutions per second, 34 revolutions per second and ranges thereof.
In a preferred embodiment, the other adjuvants include stearic acid and antioxidants.
In a preferred embodiment, the amount of the pyrolysis carbon residue is 100 parts by weight, the amount of the stearic acid is any one of 1 to 5 parts by weight, the amount of the antioxidant is any one of 0.2 to 5 parts by weight, and the amount of the polyene ester resin is any one of 1 to 8 parts by weight. Further, according to the weight parts, the cracking carbon residue is 100 parts, the stearic acid is 3 parts, the antioxidant is 3 parts, and the polyene ester resin is 5 parts.
In a preferred embodiment, the method further comprises a crushing treatment step, a magnetic separation treatment step and a cracking carbonization treatment step before the grinding modification treatment step. And removing steel wires in the rubber blocks through a magnetic separation treatment step to obtain the rubber blocks after the magnetic separation treatment.
In a preferred embodiment, the crushing step comprises: firstly, crushing the waste tires in a first section to obtain adhesive tapes, and then crushing the adhesive tapes in a second section to obtain adhesive blocks; the device used for the first-stage crushing treatment is a strip crusher, and the device used for the second-stage crushing treatment is a granular crusher; the grain diameter of the rubber block is less than or equal to 35mm. The rubber blocks with the particle size obtained by processing the waste tires can fully react in the subsequent cracking carbonization treatment and carbonization treatment, so that the surface activity of the modified cracking carbon black is further improved.
In a preferred embodiment, the step of lysing carbonization comprises: and (3) conveying the glue blocks treated by the magnetic separation treatment step into a cracking device, and carrying out cracking carbonization treatment at 380-480 ℃ to obtain the cracking carbon residue. It will be appreciated that the pyrolysis carbonization treatment temperature may also be 380 ℃, 420 ℃, 480 ℃ and any point value within its range.
The invention also provides modified cracked carbon black, which is prepared by the preparation method of the modified cracked carbon black in any one of the technical schemes. The particle size of the modified cracking carbon black is controlled between 5 and 8 mu m, so that the surface activity of the cracking carbon black is effectively improved, the dispersibility of the cracking carbon black in rubber is improved, and the modified cracking carbon black has the characteristics of excellent reinforcement and wear resistance.
In order to more clearly and in detail describe the modified cracked carbon black and the preparation method thereof provided by the embodiment of the present invention, the following description will be made with reference to specific examples.
Example 1
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 1 part of stearic acid, 0.2 part of antioxidant and 1 part of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 380 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue and the polyenoic ester resin into a mixing tank, mixing and stirring for 0.5h at the temperature of 100 ℃ to obtain a mixture A, pushing and grinding the mixture A, stearic acid and an antioxidant according to the frequency of 3Hz, and carrying out blending superfine grinding modification treatment under the condition that the grinding rotating speed is 30 r/s and the induced air rotating speed is 28 r/s.
Example 2
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 2 parts of stearic acid, 1 part of antioxidant and 2 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 420 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue and the polyenoic ester resin into a mixing tank, mixing and stirring for 0.5h at 105 ℃ to obtain a mixture A, pushing and grinding the mixture A, stearic acid and an antioxidant according to the frequency of 5Hz, and carrying out blending superfine grinding modification treatment under the condition that the grinding speed is 35 r/s and the induced air speed is 30 r/s.
Example 3
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 6 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue and the polyenoic ester resin into a mixing tank, mixing and stirring for 0.5h at 110 ℃ to obtain a mixture A, pushing and grinding the mixture A, stearic acid and an antioxidant according to 8Hz frequency, and carrying out blending superfine grinding modification treatment under the conditions that the grinding speed is 50 r/s and the induced air speed is 36 r/s.
Example 4
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 4 parts of stearic acid, 3.5 parts of antioxidant and 8 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 470 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue and the polyenoic ester resin into a mixing tank, mixing and stirring for 0.5h at 115 ℃ to obtain a mixture A, pushing and grinding the mixture A, stearic acid and an antioxidant according to the frequency of 10Hz, and carrying out blending superfine grinding modification treatment under the condition that the grinding speed is 40 r/s and the induced air speed is 32 r/s.
Example 5
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 5 parts of stearic acid, 5 parts of antioxidant and 4 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 480 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue and the polyenoic ester resin into a mixing tank, mixing and stirring for 0.5h at 120 ℃ to obtain a mixture A, pushing and grinding the mixture A, stearic acid and an antioxidant according to 8Hz frequency feed, and carrying out blending superfine grinding modification treatment under the condition that the grinding rotating speed is 45 r/s and the induced air rotating speed is 34 r/s.
Comparative example 1
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 1 part of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue, the polyenoic ester resin and the stearic acid into a mixing tank, mixing and stirring for 0.5h at 110 ℃ to obtain a mixture A, pushing and grinding the mixture A and the antioxidant according to 8Hz frequency, and carrying out blending superfine grinding modification treatment under the condition that the grinding rotating speed is 50 r/s and the induced air rotating speed is 25 r/s.
Comparative example 2
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 3 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue, the polyenoic ester resin and the antioxidant into a mixing tank, mixing and stirring for 0.5h at 110 ℃ to obtain a mixture A, pushing and grinding the mixture A and stearic acid according to 8Hz frequency, and carrying out blending superfine grinding modification treatment under the conditions that the grinding speed is 50 r/s and the induced air speed is 28 r/s.
Comparative example 3
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 2 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding blending superfine grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue, stearic acid, an antioxidant and a polyene ester resin into a mixing tank, mixing and stirring for 0.5h at 110 ℃ to obtain a mixture A, then feeding and pushing the mixture A according to 8Hz frequency, grinding, and carrying out blending superfine grinding modification treatment under the conditions that the grinding speed is 50 r/s and the induced air speed is 36 r/s.
Comparative example 4
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 6 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue, stearic acid and an antioxidant into a mixing tank, mixing and stirring for 0.5h at 110 ℃ to obtain a mixture A, pushing and grinding the mixture A and the polyenoic ester resin according to the 3Hz frequency, and carrying out blending superfine grinding modification treatment under the conditions that the grinding speed is 30 r/s and the induced air speed is 28 r/s.
Comparative example 5
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 6 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, the cracking carbon residue and the antioxidant are added into a mixing tank, mixed and stirred for 0.5h at 110 ℃ to obtain a mixture A, and then the mixture A, stearic acid and the polyene ester resin are fed and pushed according to the frequency of 5Hz and are ground, and the blending superfine grinding modification treatment is carried out under the conditions that the grinding speed is 35 r/s and the induced air speed is 30 r/s.
Comparative example 6
The embodiment provides a preparation method of blending grinding modified cracking carbon black, which comprises the following specific contents:
the blending grinding modified cracking carbon black formula comprises the following raw materials in parts by weight:
100 parts of cracking carbon residue, 3 parts of stearic acid, 2 parts of antioxidant and 6 parts of polyenoic ester resin. Wherein the polyene ester resin is LSR-395.
The preparation method of the blending grinding modified cracking carbon black comprises the following steps:
(1) Crushing: firstly, carrying out primary crushing treatment on waste tires by adopting a strip crusher to obtain rubber strips, and then carrying out secondary crushing treatment on the obtained rubber strips by adopting a granular crusher to obtain rubber blocks, wherein the grain size of the rubber blocks is less than or equal to 35mm;
(2) Magnetic separation: magnetically separating the rubber block obtained in the step (1) to remove steel wires in the rubber block, thereby obtaining a magnetically separated rubber block;
(3) And (3) cracking and carbonizing treatment: transferring the glue blocks obtained in the step (2) after the magnetic separation treatment into a cracking kettle, and carrying out cracking carbonization treatment at 450 ℃ to obtain cracking carbon residues;
(4) Grinding modification treatment: according to the weight portion ratio, firstly adding the cracking carbon residue and stearic acid into a mixing tank, mixing and stirring for 0.5h at 110 ℃ to obtain a mixture A, pushing and grinding the mixture A, the antioxidant and the polyene ester resin according to the frequency of 10Hz, and carrying out blending superfine grinding modification treatment under the conditions that the grinding speed is 45 r/s and the induced air speed is 25 r/s.
Performance testing
Prepared by using examples 1 to 5 and comparative examples 1 to 6
Table 1 chemical properties of the example and comparative example cracked carbon blacks
The modified cracking carbon black fillers prepared in examples 1-5 and comparative examples 1-6, and the waste tire cracking carbon residue without any treatment were used to prepare rubber, and the performance (waste tire cracking carbon residue without any treatment) was tested according to the national standard method, and the test results are shown in Table 2.
Table 2 properties of the example and comparative compounds
It can be seen from the above chemical property and physical property detection data that the modified cracked carbon black prepared by the method has the advantages of ultra-fine fineness, high iodine absorption value, large specific surface area, high structural degree, good dispersibility, higher reinforcing property, wear resistance and the like, and wide application prospect, and the modified cracked carbon black obtained by the method in the embodiment 3 has the best performance in the above 5 embodiments and 6 comparative embodiments, so the embodiment 3 is the best embodiment, and the variables in the range also belong to the protection scope of the scheme.
In summary, the invention provides a modified and modified cracked carbon black and a preparation method thereof, when the cracked carbon black is modified, based on the polarization characteristics of the polyenoic ester resin, the structure of the carbon black particle aggregate is destroyed by the action of mechanical shearing force during grinding, the variety and the number of surface groups are changed, the surface activity and the polarity are increased, the reagglomeration trend of the carbon black is reduced, the polyenoic ester resin is grafted to the surface of the cracked carbon black particle, and the cracked carbon black is endowed with good polarization performance, so that the compatibility with various raw materials and auxiliary materials of rubber is good, thereby obtaining a cracked carbon black product with excellent performances, solving the further application problem that the cracked carbon black product obtained by the prior cracking technology cannot be well applied due to low performance, and expanding the application range of the blended superfine grinding modified cracked carbon black in high-performance tires. The invention has the characteristics of simple preparation process, controllable cost, excellent performances of carbon black and the like.
Claims (10)
1. A method for preparing modified cracked carbon black, comprising a grinding modification treatment step, wherein the grinding modification treatment step further comprises: premixing the cracking carbon black and the polyenoic ester resin to prepare a mixture A, and grinding the mixture A and other auxiliary agents at any value of 30-50 r/s.
2. The method of producing modified, cracked carbon black according to claim 1, wherein the polyene ester resin is selected from LSR-395 resins.
3. The method for producing a modified, cracked carbon black according to claim 1, wherein the grinding modification treatment step further comprises: pushing and grinding the mixture A and other auxiliary agent feed, and sending the ground mixture A and other auxiliary agent feed to a granulating process for granulating by induced air; the feeding frequency is any value of 3-10 Hz; the induced draft rotational speed is any value of 28-36 revolutions per second.
4. The method for preparing modified cracked carbon black as claimed in claim 1, wherein the other auxiliary agents include stearic acid and an antioxidant.
5. The method for producing a modified cracked carbon black according to claim 4, wherein the amount of said cracked carbon residue is 100 parts by weight, the amount of said stearic acid is 1 to 5 parts by weight, the amount of said antioxidant is 0.2 to 5 parts by weight, and the amount of said polyene ester resin is 1 to 8 parts by weight.
6. The method for producing a modified cracked carbon black according to claim 1, wherein the premixed stirring temperature at which the cracked carbon black and the polyester resin are premixed to produce the mixture a is any one of 100 to 120 ℃ and the stirring time is 0.5h.
7. The method for producing a modified cracked carbon black according to claim 1, further comprising a crushing treatment step, a magnetic separation treatment step, and a cracking carbonization treatment step prior to the grinding modification treatment step.
8. The method for producing a modified cracked carbon black according to claim 7, wherein the crushing treatment step comprises: firstly, crushing the waste tires in a first section to obtain adhesive tapes, and then crushing the adhesive tapes in a second section to obtain adhesive blocks; the device used for the first-stage crushing treatment is a strip crusher, and the device used for the second-stage crushing treatment is a granular crusher; the grain diameter of the rubber block is less than or equal to 35mm.
9. The method for producing a modified cracked carbon black according to claim 7, wherein said step of cracking carbonization comprises: and (3) conveying the glue blocks treated by the magnetic separation treatment step into a cracking device, and carrying out cracking carbonization treatment at 380-480 ℃ to obtain the cracking carbon residue.
10. A modified, cracked carbon black prepared by the method of any one of claims 1 to 9.
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