CN116808942A - Dry granulating device and method for dry granulating cracked carbon black by adopting same - Google Patents
Dry granulating device and method for dry granulating cracked carbon black by adopting same Download PDFInfo
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Abstract
The invention relates to the technical field of cracking carbon black, and discloses a dry granulating device which comprises a feeding bin, a degassing device, a tabletting device and a shaping machine; wherein, a heating component is arranged in the feeding bin and is used for receiving and heating raw materials; the deaeration device is communicated with the feeding bin and is used for deaerating the heated raw materials; the tabletting device is connected with the degasser and is arranged at the bottom of the degasser to tablet the degassed raw materials; the shaping machine is positioned at the bottom of the tabletting device and is used for crushing the tabletted raw materials into particles. According to the dry granulating device and the granulating method, the cracked carbon black with poor quality can be reprocessed, the particle size of the cracked carbon black is reduced, the reinforcing effect of the cracked carbon black is improved, meanwhile, the reinforcing dispersion performance of the cracked carbon black is improved by adding the modifier, the oil content affecting the performance of the cracked carbon black is reduced by high-temperature dry granulating, the quality of the cracked carbon black is improved, and the performance of the cracked carbon black is further improved.
Description
Technical Field
The invention relates to the technical field of cracking carbon black, in particular to a dry granulating device and a dry granulating method of cracking carbon black by adopting the device.
Background
The waste tires in China are extremely large in production amount, the waste tires are piled together as solid wastes, the environment is seriously polluted, the health of people can be influenced even, the thermal cracking treatment of the waste tires is considered as an effective recycling treatment mode, the treatment of the products is extremely important, the thermal cracking carbon black of the waste tires is one of the thermal cracking products, and how to efficiently and reasonably utilize the waste tires is an important step in the whole recycling process.
At present, the problem of poor reinforcement and dispersibility of the cracking carbon black in rubber is difficult to use in the tire industry as a large amount of reinforcing substances in a formula, the main reason for poor reinforcement and dispersibility of the cracking carbon black in rubber is that rubber macromolecular substances in the waste tire cracking process remain, oily substances are formed on the surface of the cracking carbon black in a coating mode, the oily substances coat active points of the cracking carbon black, the problem of poor dispersion of the cracking carbon black in rubber is caused, the oily substances also cause poor hydrophilicity of the cracking carbon black, the traditional wet granulation method is difficult to apply to the cracking carbon black, and particles produced by using the wet granulation cracking carbon black are easy to generate caking and have high content of fine powder.
Therefore, it is a need for a dry granulation apparatus and method for reducing the oil content of the carbon black to be processed and improving the reinforcing and dispersing properties of the carbon black to be processed.
Disclosure of Invention
In view of the above, the invention provides a dry granulation device and a dry granulation method of the cracking carbon black by adopting the device, so as to solve the problems of high oil content, poor reinforcement and dispersibility of the existing cracking carbon black.
In order to solve the technical problems, the invention adopts the following technical scheme:
in one aspect, a dry granulation device is provided, comprising a feeding bin, a degassing device, a tabletting device and a shaping machine;
wherein, a heating component is arranged in the feeding bin and is used for receiving and heating raw materials; the degasser is communicated with the feeding bin and is used for degassing the heated raw materials; the tabletting device is connected with the degasser and arranged at the bottom of the degasser to tablet the degassed raw materials; the shaping machine is positioned at the bottom of the tabletting device and is used for crushing the tabletted raw materials into particles.
Preferably, in the dry granulation device, the feeding bin comprises a bin body and a first heat conducting layer; the bin body is used for receiving raw materials, and further preferably, a heating rod can be arranged in the bin body; the first heat conduction layer is arranged around the periphery of the bin body, and heat conduction medium is filled in the first heat conduction layer.
Preferably, in the dry granulation device, the degassing device comprises a degassing pipeline, a vacuumizing pipeline and a vacuum pump; the degassing pipeline is arranged at the bottom of the feeding bin, and an auger is arranged in the degassing pipeline and used for conveying raw materials; a filter element is arranged in the degassing pipeline and is used for filtering impurities in the raw materials; the vacuumizing pipeline is connected with the degassing pipeline; the vacuum pump is connected with the vacuumizing pipeline, and vacuum pressure is transmitted to the degassing pipeline through the vacuum pump and the vacuumizing pipeline.
Preferably, in the dry granulation device, the tabletting device comprises a compression roller, a heating rod and a conductive slip ring; the compression roller is positioned at the bottom of the degassing pipeline and is used for tabletting raw materials; the heating rod penetrates through the inside of the press roller to heat the press roller; the conductive slip ring is sleeved at the end part of the compression roller rotating shaft.
Preferably, in the dry granulation apparatus, the shaping machine includes a crusher and a screening machine; the crusher is positioned at the bottom of the compression roller device and is used for crushing the pressed raw materials into particles; the screening machine is connected to the bottom of the crusher and used for screening crushed particles, qualified particles are conveyed to a qualified product storage tank through a belt, and unqualified particles are recycled to the feeding bin for cyclic treatment.
Preferably, the dry granulation device further comprises a material balance distributor arranged between the feeding bin and the degassing device, and used for uniformly mixing the new raw materials and the recovered particles;
further preferably, a second heat conducting layer is arranged on one side of the material balance distributor, and a heat conducting medium is arranged in the second heat conducting layer;
still further preferably, the first heat conducting layer and the second heat conducting layer are both connected with a heating box, so as to realize recycling of the heat conducting medium.
In another aspect, the present invention provides a method for dry granulation of cracked carbon black using any of the above-described apparatus, comprising the steps of:
(1) Modification of the cracking carbon black: adding a modifier into the cracking carbon black, and grinding and uniformly mixing to obtain modified cracking carbon black;
(2) And conveying the modified cracked carbon black to a feeding bin for heating and deoiling treatment, then feeding the modified cracked carbon black into a degassing device for degassing treatment, carrying out high-temperature tabletting on the degassed cracked carbon black by a tabletting device, and continuously carrying out crushing granulation and screening by a shaping machine.
Preferably, in the above-mentioned dry granulation method of the cracked carbon black, the addition amount of the modifier in the step (1) is 1-15% of the mass of the cracked carbon black;
further preferably, the modifier comprises the following components in mass ratio of 2: (0.01-0.5): (0.01-0.5) a reinforcing tackifying resin, a carbon black coupling agent, and a carbon black dispersing agent;
still more preferably, the reinforcing tackifying resin comprises a mass ratio of (0.01-2): (0.01-5) a reinforcing resin and a tackifying resin.
Preferably, in the above-mentioned dry granulation method of the cracked carbon black, the grinding in the step (1) is performed in a ball mill, and the ball ratio is 1:1-3, wherein the ball milling speed is 30-50Hz/min, and the ball milling time is 10-50min.
Preferably, in the above-mentioned dry granulation method of the cracked carbon black, the blanking speed of conveying the modified cracked carbon black in the step (2) to a feeding bin is 100-800kg/h;
further preferably, the heating deoiling temperature of the feeding bin is 150-400 ℃;
further preferably, the vacuum pressure of the degassing device in the degassing treatment process is 0.1-1.0MPa;
further preferably, the high temperature tablet pressing temperature of the tablet pressing device is 150-400 ℃.
The invention provides a dry granulating device and a dry granulating method for cracking carbon black, which have the beneficial effects that compared with the prior art:
according to the dry granulating device and the granulating method, the cracked carbon black with poor quality can be reprocessed, the particle size of the cracked carbon black is reduced, the reinforcing effect of the cracked carbon black is improved, meanwhile, the reinforcing dispersion performance of the cracked carbon black is improved by adding the modifier, the oil content affecting the performance of the cracked carbon black is reduced by high-temperature dry granulating, the quality of the cracked carbon black is improved, and the performance of the cracked carbon black is further improved;
the device and the method for granulating the cracking carbon black by the dry method solve the problem that the cracking carbon black cannot be granulated by the traditional dry method for granulating the carbon black, namely the method for granulating the cracking carbon black with low cost is provided, and the quality of the cracking carbon black can be improved through the granulating process;
the cracking carbon black particles obtained by the dry granulating device and the granulating method have excellent performance and high synthesis degree of the processing technology, solve the problem of high back and forth transportation and storage cost caused by stepwise processing of first production, then modification and granulation in the existing cracking carbon black production process, and can continuously modify and process the cracking carbon black with high processing efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a dry granulation apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a degasser according to an embodiment of the invention;
FIG. 3 is a schematic view of a feed bin according to an embodiment of the invention;
FIG. 4 is a schematic view of an embodiment of the present invention of a milling modification apparatus;
fig. 5 is a schematic view of a heating cabinet according to an embodiment of the present invention.
In the figure:
100-feeding bin, 110-bin body, 120-first heat conduction layer, 130-heating rod, 200-degasser, 210-degasser pipeline, 211-auger, 212-filter element, 220-vacuumizing pipeline, 230-vacuum pump, 300-tabletting device, 310-compression roller, 320-conductive slip ring, 400-shaper, 410-crusher, 420-screening machine, 500-balance distributor, 510-second heat conduction layer, 600-heating box and 700-grinding modification equipment.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1, an embodiment of the present invention provides a dry granulation apparatus, including a feed bin 100, a degasser 200, a tabletting apparatus 300, and a shaper 400;
wherein, a heating component is arranged in the feeding bin 100 and is used for receiving and heating raw materials; the degasser 200 is communicated with the feeding bin 100 and is used for degassing the heated raw materials;
the tabletting device 300 is connected with the degassing device 200 and is arranged at the bottom of the degassing device 200 so as to tablet the degassed raw materials; the shaper 400 is located at the bottom of the tabletting device 300 and is used for crushing the tabletting raw materials into particles.
When the dry granulating device is applied to dry granulating of the cracking carbon black, the heating function of the feeding bin 100 is beneficial to granulating of the cracking carbon black, and the oil contained in the feeding bin is volatilized through high Wen Daliang, so that the aim of reducing the oil content in the cracking carbon black is fulfilled; the degasser 200 can effectively improve the light-heavy density of the powder carbon black, improve the granulating effect, and volatilize the impurities, solvents and other small molecular substances adsorbed on the surface of the cracked carbon black at high temperature and then discharge the volatile substances out of the granulating system.
As shown in fig. 3, in some embodiments of the present invention, a feed bin 100 includes a bin body 110 and a first thermally conductive layer 120; the bin body 110 is configured to receive a raw material, the first heat-conducting layer 120 is disposed around the bin body 110, and a heat-conducting medium is filled in the first heat-conducting layer 120, and the heat-conducting medium may be heat-conducting oil, and is configured to heat the raw material.
Further, a heating rod 130 may be disposed in the bin body 110, because the heat conducting medium is coated on the outer side of the bin body 110, when the feeding amount of the raw materials is large, a large temperature difference may exist between the interior of the bin and a portion close to the first heat conducting layer 120, and at this time, the raw materials in the bin can be heated by the heating rod 130, so as to keep the raw materials in the bin heated uniformly;
further, the bin body 110 can be of a straight cylinder type or a funnel type, preferably of a funnel type, so that the volume of the bin body 110 can be increased, the blanking speed can be increased, and the blocking condition is avoided; and the blanking speed of the feeding bin 100 is controlled and regulated by an automatic butterfly valve.
As shown in fig. 2, in some embodiments of the invention, degasser 200 includes a degasser line 210, a vacuum line 220, and a vacuum pump 230; wherein the degassing pipeline 210 is arranged at the bottom of the feeding bin 100, and a packing auger 211 is arranged in the degassing pipeline 210 and used for conveying raw materials; a filter element 212 is arranged in the degassing pipeline 210 and is used for filtering impurities in the raw materials; the vacuum line 220 is connected to the degassing line 210; the vacuum pump 230 is connected with the vacuumizing pipeline 220, and vacuum pressure is transmitted to the degassing pipeline 210 through the vacuum pump 230 and the vacuumizing pipeline 220 so as to remove impurities, solvents and other small molecular substances adsorbed on the surface of the cracked carbon black.
In some embodiments of the present invention, sheeting apparatus 300 includes a press roller 310, a heating rod 130, and an electrically conductive slip ring 320; wherein, the compression roller 310 is positioned at the bottom of the degassing pipeline 210 and is used for tabletting raw materials; the heating rod 130 penetrates through the inside of the press roller 310 to heat the press roller 310, and high-temperature treatment is carried out on the raw materials in the tabletting process, so that the dispersibility of the raw materials is effectively improved; the conductive slip ring 320 is sleeved at the end of the rotating shaft of the pressing roller 310 and is used for providing power for the transmission device and the heating device.
In some embodiments of the present invention, the shaper 400 includes a crusher 410 and a screening machine 420; wherein the crusher 410 is positioned at the bottom of the press roll 310 device and is used for crushing the pressed raw materials into particles; the screening machine 420 is connected to the bottom of the crusher 410, and is used for screening crushed particles, qualified particles are conveyed to a qualified product storage tank through a belt, and unqualified particles are recovered to the feeding bin 100 for cyclic treatment.
Specifically, when the dry granulation device is applied to the cracking of carbon black, the shaping machine 400 has the function of uniformly crushing the flaked cracking carbon black into particles, and the hardness of the particles is between 30 and 80 after the particles are screened by the screening machine 420, and the unqualified cracking carbon black is recycled and then is participated in granulation again.
In some embodiments of the present invention, the apparatus further comprises a material balance distributor 500 disposed between the feeding bin 100 and the degassing device 200, for uniformly mixing the new raw materials and the recovered particles; further, a second heat conducting layer 510 is arranged on one side of the material balance distributor 500, and a heat conducting medium is arranged in the second heat conducting layer 510, wherein the heat conducting medium is preferably heat conducting oil, so that the raw materials are properly insulated, and the cooling speed of the raw materials is reduced;
it can be understood that the first heat conducting layer 120 and the second heat conducting layer 510 are both provided with an inlet and an outlet, and are connected to the heating box 600 through the inlet and the outlet, as shown in fig. 5, the heating box 600 is internally provided with the heating rod 130 to realize cyclic utilization of heat conducting media, and when the heat conducting media of the first heat conducting layer 120 and the second heat conducting layer 510 are the same, the two heat conducting layers can share one heating box 600, and the heating box 600 is provided with an oil inlet and an oil outlet, the oil inlet of the heating box 600 is respectively communicated with the oil outlets of the first heat conducting layer 120 and the second heat conducting layer 510, and the oil outlet of the heating box 600 is respectively communicated with the oil inlets of the first heat conducting layer 120 and the second heat conducting layer 510 to form a circulation loop, so as to realize cyclic utilization of the heat conducting media.
As shown in fig. 4, in some embodiments of the present invention, the apparatus further includes a grinding and modifying apparatus 700 connected to the feed inlet of the feed bin 100, and when the raw materials need to be modified, the raw materials are first modified by the grinding and modifying apparatus 700 and ground to a certain particle size, and then are transported to the feed bin 100 for subsequent processing.
The dry granulating device can continuously modify and subsequently process the raw materials, does not need to bear higher transportation and storage cost, improves the performance of the raw materials, improves the processing efficiency, and is suitable for industrial production.
In addition, in other embodiments of the present invention, there is provided a method of dry granulation of cracked carbon black using any of the apparatus described above, comprising the steps of:
s100, modification of the cracking carbon black: adding a modifier into the cracking carbon black, and grinding and uniformly mixing to obtain modified cracking carbon black;
the reinforcing dispersion performance of the cracking carbon black is improved by adding the modifier, wherein the addition amount of the modifier is 1-15%, preferably 1-10%, more preferably 2-8%, for example, 2%, 5%, 8% and the like of the mass of the cracking carbon black;
further, the modifier comprises the following components in percentage by mass: (0.01-0.5): (0.01-0.5) a reinforcing tackifying resin, a carbon black coupling agent, and a carbon black dispersing agent; the carbon black coupling agent comprises but is not limited to a silane coupling agent and a titanate coupling agent, and the carbon black dispersing agent comprises but is not limited to a styrene-butadiene-styrene copolymer (SBS), polymethyl methacrylate (PMMA) and polyvinyl alcohol (PVA), and is mainly used for improving the dispersion performance of the cracked carbon black, avoiding the agglomeration phenomenon in the subsequent rubber preparation process, and improving the mechanical properties such as strength, hardness, wear resistance and the like; and the mass ratio of the reinforcing tackifying resin, the carbon black coupling agent and the carbon black dispersing agent in the modifier can be 2:0.01:0.5, 2:0.01:0.01, 2:0.01-0.3, 2:0.3:0.2, etc., and specifically can be adjusted within this range according to the actual situation.
Still further, the reinforcing tackifying resin comprises a mass ratio of (0.01-2): (0.01-5) a reinforcing resin and a tackifying resin, the mass ratio of the reinforcing resin to the tackifying resin may be 1: 1. 2:0.01, 0.01: 2. 0.05:5, etc. for improving the reinforcing performance of the cracked carbon black and improving the quality of the cracked carbon black.
Further, the grinding in the step (1) is performed in a ball mill, and the ball ratio of the grinding machine is 1:1-3, wherein the ball milling speed is 30-50Hz/min, and the ball milling time is 10-50min. The dispersion performance of the cracked carbon black can be improved to a certain extent by controlling the proper ball ratio, ball milling speed and ball milling time.
And S200, conveying the modified cracked carbon black to a feeding bin 100 for heating and deoiling treatment, then feeding the modified cracked carbon black into a degassing device 200 for degassing treatment, tabletting the degassed cracked carbon black at a high temperature by a tabletting device 300, and continuously crushing, granulating and screening by a shaping machine 400.
The step adopts high-temperature dry granulation, so that the oil content in the cracked carbon black can be effectively reduced, which is equivalent to the secondary cracking process, and the quality performance of the cracked carbon black can be further improved.
Further, the unloading speed of the modified cracked carbon black in the step (2) to the feeding bin 100 is 100-800kg/h, preferably 150-600kg/h, more preferably 200-500kg/h, for example, 200kg/h, 350kg/h, 500kg/h and the like, the dry granulation process can be kept continuously, the transportation and storage cost is reduced, and the unloading speed can be kept to ensure that the impurity removal in the subsequent degassing process is more complete and the tabletting thickness is moderate;
further, the heating deoiling temperature of the feeding bin 100 is 150 to 400 ℃, for example, 150 ℃, 300 ℃, 400 ℃ and the like, and oily substances coated on the surface of the cracked carbon black are removed by high-temperature heating treatment, so that the dispersibility of the cracked carbon black is improved.
Further, the vacuum pressure of the degasser 200 in the degasification process is 0.1-1.0MPa, for example, 0.1MPa, 0.5MPa, 1.0MPa, etc., impurities and solvents on the surface of the cracked carbon black can be removed by degasification, the purity of the product is improved, and the dry granulation device can be in a negative pressure environment by vacuumizing to obtain the cracked carbon black with proper granularity, so that the dispersion performance is enhanced.
Further, the high temperature of the tabletting device 300 is 150-400 ℃, such as 150 ℃, 300 ℃, 400 ℃ and the like, and the cracked carbon black is kept in a higher temperature state in the dry granulating process, so that the granulating effect of the cracked carbon black is improved, and the reinforcing and dispersing performances of the cracked carbon black are improved.
The dry granulation process of the cracked carbon black of the present invention is described in detail below with reference to specific examples.
Example 1
The embodiment provides a dry granulation method for cracking carbon black, which comprises the following steps:
(1) The cracking carbon black is subjected to air grinding and superfine grinding, and the power of a main grinding machine is 50Hz;
(2) Adding 8% of modifier into the cracked carbon black, uniformly mixing the cracked carbon black added with the modifier in a conical mixing device, and then grinding and uniformly mixing the mixture in a grinding machine for 20min at a ball milling speed of 30Hz/min, so that the modifier and the cracked carbon black undergo a grafting reaction in the grinding process to obtain the modified cracked carbon black; wherein the modifier comprises the following components in percentage by mass: 0.3:0.05 of a reinforcing tackifying resin, a silane coupling agent KH-550 and a styrene-butadiene-styrene copolymer; the reinforcing tackifying resin comprises the following components in percentage by mass: 1, a tall oil modified phenolic reinforcing resin and an octyl phenolic tackifying resin, wherein the ball ratio of the grinder is 1:1-3;
(3) Adding the modified cracked carbon black into a dry granulating device, controlling the feeding speed to be 450kg/h, conveying the cracked carbon black to a feeding bin, treating at 250 ℃, then feeding the treated cracked carbon black into a degassing device, setting the vacuum pump pressure of the degassing device to be 0.6MPa, feeding the degassed cracked carbon black into a compression roller, tabletting at the high temperature of 250 ℃, enabling the speed of a compression roller motor to be 50Hz, feeding the tablet cracked carbon black into a shaping machine, uniformly crushing the tablet cracked carbon black into particles, screening to obtain qualified particles with the hardness of 40-70, and recycling the unqualified particles into the feeding bin for re-granulation.
Example 2
The embodiment provides a dry granulation method for cracking carbon black, which comprises the following steps:
(1) The cracking carbon black is subjected to air grinding and superfine grinding, and the power of a main grinding machine is 20Hz;
(2) Adding 3% of modifier into the cracked carbon black, uniformly mixing the cracked carbon black added with the modifier in a conical mixing device, and then grinding and uniformly mixing the mixture in a grinding machine for 30min at a ball milling speed of 40Hz/min, so that the modifier and the cracked carbon black undergo a grafting reaction in the grinding process to obtain the modified cracked carbon black; wherein the modifier comprises the following components in percentage by mass: 0.01:0.5 of a reinforcing tackifying resin, a silane coupling agent KH-560 and polymethyl methacrylate; the reinforcing tackifying resin comprises the following components in percentage by mass of 0.01:5, a tall oil modified phenolic reinforcing resin and a cayenne tackifying resin, wherein the ball ratio of the grinder is 1:1-3;
(3) Adding the modified cracked carbon black into a dry granulating device, controlling the feeding speed to be 600kg/h, conveying the cracked carbon black to a feeding bin, treating at 150 ℃, then feeding the treated cracked carbon black into a degassing device, setting the vacuum pump pressure of the degassing device to be 0.3MPa, feeding the degassed cracked carbon black into a compression roller, tabletting at the high temperature of 150 ℃, wherein the speed of a motor of the compression roller is 10Hz, feeding the tablet cracked carbon black into a shaping machine, uniformly crushing the tablet cracked carbon black into particles, screening to obtain qualified particles with the hardness of 40-70, and recycling the unqualified particles into the feeding bin for re-granulation.
Example 3
The embodiment provides a dry granulation method for cracking carbon black, which comprises the following steps:
(1) The cracking carbon black is subjected to air grinding and superfine grinding, and the power of a main grinding machine is 80Hz;
(2) Adding 1% of modifier into the cracked carbon black, uniformly mixing the cracked carbon black added with the modifier in a conical mixing device, and then grinding and uniformly mixing the mixture in a grinding machine for 10min at a ball milling speed of 50Hz/min, so that the modifier and the cracked carbon black undergo a grafting reaction in the grinding process to obtain the modified cracked carbon black; wherein the modifier comprises the following components in percentage by mass: 0.02:0.01 of reinforced tackifying resin, a silane coupling agent KH570 and polyvinyl alcohol; the reinforcing tackifying resin comprises the following components in percentage by mass: 0.01 of high styrene resin and tertiary butyl tackifying resin, the ball ratio of the grinder is 1:1-3;
(3) Adding the modified cracked carbon black into a dry granulating device, controlling the feeding speed to be 100kg/h, conveying the cracked carbon black to a feeding bin, treating at 300 ℃, then feeding the treated cracked carbon black into a degassing device, setting the vacuum pump pressure of the degassing device to be 1.0MPa, feeding the degassed cracked carbon black into a compression roller, tabletting at the high temperature of 300 ℃, controlling the speed of a motor of the compression roller to be 30Hz, feeding the tablet cracked carbon black into a shaping machine, uniformly crushing the tablet cracked carbon black into particles, screening to obtain qualified particles with the hardness of 40-70, and recycling the unqualified particles into the feeding bin for re-granulation.
Example 4
The embodiment provides a dry granulation method for cracking carbon black, which comprises the following steps:
(1) The cracking carbon black is subjected to air grinding and superfine grinding, and the power of a main grinding machine is 100Hz;
(2) Adding 15% of modifier into the cracked carbon black, uniformly mixing the cracked carbon black added with the modifier in a conical mixing device, and then grinding and uniformly mixing the mixture in a grinding machine for 50min at a ball milling speed of 35Hz/min, so that the modifier and the cracked carbon black undergo a grafting reaction in the grinding process to obtain the modified cracked carbon black; wherein the modifier comprises the following components in percentage by mass: 0.4:0.09 reinforcing tackifying resin, titanate coupling agent and polyvinyl alcohol; the reinforcing tackifying resin comprises the following components in percentage by mass of 0.5:3.2 high styrene resin and octyl phenol tackifying resin, ball ratio of mill is 1:1-3;
(3) Adding the modified cracked carbon black into a dry granulating device, controlling the feeding speed to be 800kg/h, conveying the cracked carbon black to a feeding bin, treating at 400 ℃, then feeding the treated cracked carbon black into a degassing device, setting the vacuum pump pressure of the degassing device to be 0.1MPa, feeding the degassed cracked carbon black into a compression roller, tabletting at the high temperature of 400 ℃, enabling the speed of a compression roller motor to be 60Hz, feeding the tablet cracked carbon black into a shaping machine, uniformly crushing the tablet cracked carbon black into particles, screening to obtain qualified particles with the hardness of 40-70, and recycling the unqualified particles into the feeding bin for re-granulation.
The steps for preparing vulcanized rubber by using the cracked carbon black particles of examples 1-4 are as follows: mixing the cracked carbon black particles with natural rubber, stearic acid, zinc oxide, accelerator DM and sulfur according to a proportion of 50:100:3:5:0.6:2.5, mixing rubber, and vulcanizing at 145 ℃ to obtain vulcanized rubber.
The physical properties of the cracked carbon black particles obtained in examples 1 to 4, and the physical properties of the vulcanized gums prepared from the cracked carbon black particles of examples 1 to 4 were measured, and the results are shown in Table 1:
TABLE 1
Comparative example 1
This comparative example is substantially identical to example 1, with the only difference that: and (3) adding 0.5% of modifier in the step (2).
Comparative example 2
This comparative example is substantially identical to example 1, with the only difference that: 16% of modifier is added in the step (2).
Comparative example 3
This comparative example is substantially identical to example 1, with the only difference that: 20% of modifier is added in the step (2).
The physical properties of the cracked carbon black particles obtained in comparative examples 1 to 3, and the physical properties of the vulcanized rubber prepared from the cracked carbon black particles of comparative examples 1 to 3 were measured, and the results are shown in Table 2:
TABLE 2
As is clear from Table 2, the addition of the modifier can greatly improve the dispersion and reinforcement properties of the cracked carbon black, and the tensile strength and 300% elongation stress properties of the cracked carbon black in rubber after the modifier is used are improved. When the addition amount of the modifier is too small, the modified cracking carbon black has poor dispersion performance and reinforcing performance and higher ash value; when the addition amount is too large, the properties of the modified cracking carbon black and the rubber properties are not changed greatly, and the ash value is increased, so that the addition amount of the modifier is 1-15% of the mass of the cracking carbon black.
Comparative example 4
This comparative example is substantially identical to example 1, with the only difference that: the mass ratio of the modifier in the step (2) is 0.3: silane coupling agent KH-550 and styrene-butadiene-styrene copolymer of 0.05 was not involved in the addition of the reinforcing tackifying resin.
Comparative example 5
This comparative example is substantially identical to example 1, with the only difference that: in the step (2), the mass ratio of the modifier is 2:0.3:0.05 tall oil modified phenolic reinforcing resin, silane coupling agent KH-550 and styrene-butadiene-styrene copolymer, no addition of tackifying resin was involved.
Comparative example 6
This comparative example is substantially identical to example 1, with the only difference that: in the step (2), the mass ratio of the modifier is 2:0.3:0.05 octyl phenol tackifying resin, silane coupling agent KH-550 and styrene-butadiene-styrene copolymer, no reinforcing resin addition was involved.
Comparative example 7
This comparative example is substantially identical to example 1, with the only difference that: the modifier in the step (2) comprises the following components in percentage by mass: 0.3:0.05 of a reinforcing tackifying resin, a silane coupling agent KH-550 and a styrene-butadiene-styrene copolymer; the reinforcing tackifying resin comprises the following components in percentage by mass: 1 and octyl phenolic tackifying resins.
The physical properties of the cracked carbon black particles obtained in comparative examples 4 to 7, and the physical properties of the vulcanized rubbers prepared from the cracked carbon black particles of comparative examples 4 to 7 were measured, and the results are shown in Table 3:
TABLE 3 Table 3
As shown in Table 3, the modifier can greatly improve the dispersion performance and reinforcing performance of the modified carbon black, and the tensile strength and 300% stress performance of the modified carbon black in rubber are improved. When the type of the modifier or the preparation proportion is changed, the mechanical property of the vulcanized rubber can be greatly influenced.
Comparative example 8
This comparative example is substantially identical to example 1, with the only difference that: and (3) conveying the modified cracked carbon black in the step (3) to a feeding bin at a blanking speed of 50kg/h.
Comparative example 9
This comparative example is substantially identical to example 1, with the only difference that: and (3) conveying the modified cracked carbon black in the step (3) to a feeding bin at a blanking speed of 900kg/h.
Comparative example 10
This comparative example is substantially identical to example 1, with the only difference that: and (3) conveying the modified cracked carbon black in the step (3) to a feeding bin at a feeding speed of 1000kg/h.
The physical properties of the cracked carbon black particles obtained in comparative examples 8 to 10, and the physical properties of the vulcanized rubber prepared from the cracked carbon black particles of comparative examples 8 to 10 were measured, and the results are shown in Table 4:
TABLE 4 Table 4
As is clear from Table 4, the feeding speed mainly affects the quality of the particles of the modified and pelletized carbon black, and if the feeding speed is low, the particles are unevenly pelletized, the crushing strength is low, the content of fine powder is too high, and if the feeding speed is high, the properties of the particles are not changed greatly, but the energy consumption is increased, so that the feeding speed is comprehensively considered to be 100-800kg/h.
Comparative example 11
This comparative example is substantially identical to example 1, with the only difference that: and conveying the cracked carbon black to a feeding bin and then treating the cracked carbon black at normal temperature.
Comparative example 12
This comparative example is substantially identical to example 1, with the only difference that: the cracked carbon black is transported to a feed bin and then treated at 100 ℃.
Comparative example 13
This comparative example is substantially identical to example 1, with the only difference that: the cracked carbon black is transported to a feed bin and then treated at 450 ℃.
Comparative example 14
This comparative example is substantially identical to example 1, with the only difference that: the cracked carbon black is transported to a feed bin and then treated at 550 ℃.
The physical properties of the cracked carbon black particles obtained in comparative examples 11 to 14, and the physical properties of the vulcanized gums prepared by cracking the carbon black particles in comparative examples 11 to 14 were measured, and the results are shown in Table 5:
TABLE 5
As shown in Table 5, the heating deoiling can effectively improve the granulation quality and the reinforcing effect of the modified cracked carbon black, the particle crushing strength distribution is more uniform, and the tensile strength performance and the stretching stress of the vulcanized rubber prepared by the modified cracked carbon black are improved.
Comparative example 15
This comparative example is substantially identical to example 1, with the only difference that: in the step (3), the modified cracked carbon black is not subjected to degassing treatment.
Comparative example 16
This comparative example is substantially identical to example 1, with the only difference that: the vacuum pressure of the degasser during the degassing treatment is 1.2MPa.
Comparative example 17
This comparative example is substantially identical to example 1, with the only difference that: the vacuum pressure of the degasser during the degassing treatment is 1.5MPa.
The physical properties of the cracked carbon black particles obtained in comparative examples 15 to 17, and the physical properties of the vulcanized rubber prepared by cracking the carbon black particles in comparative examples 15 to 17 were measured, and the results are shown in Table 6:
TABLE 6
As can be seen from Table 6, the vacuum degassing is effective in discharging high temperature volatile substances, reducing ash content of the cracked carbon black, and improving tensile strength and 300% elongation stress of the vulcanized rubber. According to the research, if the vacuum degassing is not performed, even if the heating deoiling treatment is performed, the effective granulation is difficult, and the granulation yield of the cracking carbon black is lower, which is only 40-60%; after heating deoiling and vacuum degassing treatment, ash content can be effectively reduced, and mechanical properties of vulcanized rubber can be enhanced; the vacuum degassing pressure is limited to be 0.1-1MPa because various performances of the vacuum degassing pressure cannot be obviously improved after the vacuum degassing pressure exceeds 1MPa.
Comparative example 18
This comparative example is substantially the same as example 1 except that tabletting is performed at normal temperature.
Comparative example 19
This comparative example is substantially the same as example 1 except that the high temperature lamination temperature is 100 ℃.
Comparative example 20
This comparative example is substantially the same as example 1 except that the high temperature lamination temperature is 450 ℃.
The physical properties of the cracked carbon black particles obtained in comparative examples 18 to 20, and the physical properties of the vulcanized rubber prepared from the cracked carbon black particles of comparative examples 18 to 20 were measured, and the results are shown in Table 7:
TABLE 7
As shown in Table 6, the higher the tabletting temperature is, the better the performance of the modified cracked carbon black and the performance of the vulcanized rubber are, but when the tabletting temperature reaches a certain value, the performance improvement is not great, the comprehensive consideration of energy consumption limits the tabletting temperature to 150-400 ℃, and compared with normal-temperature tabletting, the tabletting can effectively improve the granulating effect of the cracked carbon black under the heating condition, the particle shape is more uniform, and the dispersibility is better.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the solution disclosed in the embodiments, since it corresponds to the method disclosed in the embodiments, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A dry granulation apparatus, comprising:
the feeding bin is internally provided with a heating component for receiving and heating raw materials;
the deaeration device is communicated with the feeding bin and is used for deaerating the heated raw materials;
the tabletting device is connected with the degassing device and arranged at the bottom of the degassing device so as to tablet the degassed raw materials;
and the shaping machine is positioned at the bottom of the tabletting device and is used for crushing the tabletted raw materials into particles.
2. The dry granulation apparatus as set forth in claim 1, wherein said feed bin comprises:
the bin body is used for receiving raw materials;
the first heat conduction layer is arranged around the periphery of the bin body, and heat conduction medium is filled in the first heat conduction layer.
3. Dry granulation device according to claim 1, characterized in that said degassing device comprises:
the degassing pipeline is arranged at the bottom of the feeding bin, and a packing auger is arranged in the degassing pipeline and used for conveying raw materials; a filter element is arranged in the degassing pipeline and is used for filtering impurities in the raw materials;
the vacuumizing pipeline is connected with the degassing pipeline;
and the vacuum pump is connected with the vacuumizing pipeline and transmits vacuum pressure to the degassing pipeline through the vacuum pump and the vacuumizing pipeline.
4. A dry granulation apparatus as claimed in claim 3, wherein the tabletting apparatus comprises:
the compression roller is positioned at the bottom of the degassing pipeline and is used for tabletting raw materials;
the heating rod penetrates through the inside of the press roller to heat the press roller;
and the conductive slip ring is sleeved at the end part of the compression roller rotating shaft.
5. The dry granulation apparatus according to claim 4, wherein the shaper comprises
The crusher is positioned at the bottom of the compression roller device and is used for crushing the pressed raw materials into particles;
and the screening machine is connected to the bottom of the crusher and used for screening crushed particles, qualified particles are conveyed to a qualified product storage tank through a belt, and unqualified particles are recycled to the feeding bin for cyclic treatment.
6. The dry granulation device according to claim 2, further comprising a material balance distributor disposed between the feed bin and the degasser for performing a blending operation on the fresh raw material and the recovered particles;
and/or one side of the material balance distributor is provided with a second heat conduction layer, and a heat conduction medium is arranged in the second heat conduction layer;
and/or the first heat conduction layer and the second heat conduction layer are connected with a heating box so as to realize the recycling of the heat conduction medium.
7. A process for dry granulation of carbon black by means of a device according to any one of claims 1 to 6, characterized in that it comprises the following steps:
(1) Modification of the cracking carbon black: adding a modifier into the cracking carbon black, and grinding and uniformly mixing to obtain modified cracking carbon black;
(2) And conveying the modified cracked carbon black to a feeding bin for heating and deoiling treatment, then feeding the modified cracked carbon black into a degassing device for degassing treatment, carrying out high-temperature tabletting on the degassed cracked carbon black by a tabletting device, and continuously carrying out crushing granulation and screening by a shaping machine.
8. The method for dry granulation of a carbon black according to claim 7, wherein the modifier is added in the amount of 1 to 15% of the mass of the carbon black to be granulated;
and/or the modifier comprises the components with the mass ratio of 2: (0.01-0.5): (0.01-0.5) a reinforcing tackifying resin, a carbon black coupling agent, and a carbon black dispersing agent;
and/or the reinforcing tackifying resin comprises (0.01-2) by mass: (0.01-5) a reinforcing resin and a tackifying resin.
9. The method for dry granulation of cracked carbon black according to claim 7, wherein the grinding in step (1) is performed in a ball mill with a ball ratio of 1:1-3, wherein the ball milling speed is 30-50Hz/min, and the ball milling time is 10-50min.
10. The method for dry granulation of cracked carbon black according to claim 7, wherein the blanking speed of the modified cracked carbon black in the step (2) to the feeding bin is 100-800kg/h;
and/or the heating deoiling temperature of the feeding bin is 150-400 ℃;
and/or the vacuum pressure of the degassing device in the degassing treatment process is 0.1-1.0MPa;
and/or the high temperature tablet pressing temperature of the tablet pressing device is 150-400 ℃.
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