A dry granulation device and a method for dry granulation of pyrolysis carbon black using the device

Abstract

The present invention relates to the technical field of pyrolysis carbon black, and discloses a dry granulation device, including a feed bin, a degassing device, a tabletting device and a shaping machine; wherein a heating component is arranged in the feed bin, for receiving and heating raw materials; the degassing device is connected to the feed bin, for degassing the heated raw materials; the tabletting device is connected to the degassing device, and is arranged at the bottom of the degassing device to tablet the degassed raw materials; the shaping machine is located at the bottom of the tabletting device, for crushing the tabletted raw materials into particles. The dry granulation device and granulation method of the present invention can reprocess the pyrolysis carbon black of poor quality, reduce the particle size of the pyrolysis carbon black, and improve the reinforcement effect of the pyrolysis carbon black. At the same time, the reinforcing and dispersing performance of the pyrolysis carbon black is improved by adding a modifier, and the oil content that affects the performance of the pyrolysis carbon black is reduced by high-temperature dry granulation, which is equivalent to secondary pyrolysis, thereby improving the quality of the pyrolysis carbon black and further improving the performance of the pyrolysis carbon black.

Description

Technical Field

[0001] The invention relates to the technical field of cracking carbon black, in particular to a dry granulation device and a cracking carbon black dry granulation method using the device. Background Art

[0002] my country produces a huge amount of waste tires. They are piled up as solid waste, seriously polluting the environment and even affecting people's health. The thermal cracking treatment of waste tires is considered to be an effective recycling treatment method, and the treatment of its products is extremely important. Waste tire thermal cracking carbon black is one of the products of thermal cracking. How to use it efficiently and reasonably is a crucial step in the entire recycling process.

[0003] At present, pyrolysis carbon black is difficult to be used in large quantities as a reinforcing material in the tire industry due to its poor reinforcement and dispersibility in rubber. The main reason for the poor reinforcement and dispersibility of pyrolysis carbon black in rubber is that there are residual rubber macromolecules in the pyrolysis process of waste tires, which are coated on the surface of pyrolysis carbon black to form oily substances. These oily substances cover the active points of pyrolysis carbon black, causing the problem of poor dispersion of pyrolysis carbon black in rubber. These oily substances also lead to poor hydrophilicity of pyrolysis carbon black. Traditional wet granulation methods are difficult to apply to pyrolysis carbon black. Particles produced by wet granulation of pyrolysis carbon black are prone to agglomeration and high content of fine powder.

[0004] Therefore, how to provide a dry granulation device and method to reduce the oil content of pyrolysis carbon black and improve the reinforcement and dispersibility of pyrolysis carbon black is an urgent problem to be solved by those skilled in the art. Summary of the invention

[0005] In view of this, the present invention provides a dry granulation device and a pyrolysis carbon black dry granulation method using the device to solve the problems of high oil content, poor reinforcement and dispersibility of existing pyrolysis carbon black.

[0006] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0007] In one aspect, a dry granulation device is provided, comprising a feed bin, a degassing device, a tablet pressing device and a shaping machine;

[0008] Among them, a heating component is provided in the feed bin for receiving and heating the raw materials; the degassing device is connected to the feed bin for degassing the heated raw materials; the tableting device is connected to the degassing device and is arranged at the bottom of the degassing device to tablet the degassed raw materials; the shaping machine is located at the bottom of the tableting device and is used to crush the tableted raw materials into particles.

[0009] Preferably, in the above-mentioned dry granulation device, the feed bin includes a bin body and a first heat-conducting layer; the bin body is used to receive raw materials, and further preferably, a heating rod may be arranged in the bin body; the first heat-conducting layer is arranged around the periphery of the bin body, and the first heat-conducting layer is filled with a heat-conducting medium.

[0010] Preferably, in the above-mentioned dry granulation device, the degassing device includes a degassing pipeline, a vacuum pipeline and a vacuum pump; wherein the degassing pipeline is arranged at the bottom of the feed bin, and an auger is arranged in the degassing pipeline for conveying raw materials; and a filter element is arranged in the degassing pipeline for filtering out impurities in the raw materials; the vacuum pipeline is connected to the degassing pipeline; the vacuum pump is connected to the vacuum pipeline, and the vacuum pressure is transmitted to the degassing pipeline through the vacuum pump and the vacuum pipeline.

[0011] Preferably, in the above-mentioned dry granulation device, the tableting device includes a pressing roller, a heating rod and a conductive slip ring; wherein the pressing roller is located at the bottom of the degassing pipeline and is used for tableting the raw material; the heating rod runs through the inside of the pressing roller to heat the pressing roller; the conductive slip ring is sleeved on the end of the rotating shaft of the pressing roller.

[0012] Preferably, in the above-mentioned dry granulation device, the shaping machine includes a crusher and a screening machine; wherein the crusher is located at the bottom of the pressing roller device, and is used to crush the raw materials after tableting into particles; the screening machine is connected to the bottom of the crusher, and is used to screen the crushed particles, and the qualified particles are transported to the qualified product storage tank by a belt, and the unqualified particles are recovered to the feed bin for recycling treatment.

[0013] Preferably, in the above-mentioned dry granulation device, it also includes a material balance distributor, which is arranged between the feed bin and the degassing device and is used to mix the new raw materials and the recycled particles;

[0014] Further preferably, a second heat-conducting layer is provided on one side of the material balanced distributor, and a heat-conducting medium is provided in the second heat-conducting layer;

[0015] More preferably, the first heat-conducting layer and the second heat-conducting layer are both connected to a heating box to achieve recycling of the heat-conducting medium.

[0016] On the other hand, the present invention provides a method for dry granulation of pyrolysis carbon black using any of the above-mentioned devices, comprising the following steps:

[0017] (1) Pyrolysis carbon black modification: adding a modifier to the pyrolysis carbon black, grinding and mixing, and obtaining modified pyrolysis carbon black;

[0018] (2) The modified pyrolysis carbon black is transported to a feed bin for heating and deoiling, and then enters a degassing device for degassing. The degassed pyrolysis carbon black is tableted at high temperature in a tableting device, and then crushed, granulated, and screened in a shaping machine.

[0019] Preferably, in the above-mentioned dry granulation method of pyrolysis carbon black, the amount of the modifier added in step (1) is 1-15% of the mass of the pyrolysis carbon black;

[0020] Further preferably, the modifier comprises a reinforcing tackifying resin, a carbon black coupling agent and a carbon black dispersant in a mass ratio of 2:(0.01-0.5):(0.01-0.5);

[0021] More preferably, the reinforcing and tackifying resin comprises a reinforcing resin and a tackifying resin in a mass ratio of (0.01-2):(0.01-5).

[0022] Preferably, in the above-mentioned dry granulation method of pyrolysis carbon black, the grinding in step (1) is carried out in a ball mill, the material-ball ratio is 1:1-3, the ball milling speed is 30-50 Hz / min, and the ball milling time is 10-50 min.

[0023] Preferably, in the above-mentioned pyrolysis carbon black dry granulation method, the feed rate of the modified pyrolysis carbon black in step (2) to the feed bin is 100-800 kg / h;

[0024] Further preferably, the heating and deoiling temperature of the feed bin is 150-400°C;

[0025] Further preferably, the vacuum pressure of the degassing device during the degassing process is 0.1-1.0 MPa;

[0026] Further preferably, the high temperature tableting temperature of the tableting device is 150-400°C.

[0027] The present invention provides a dry granulation device and a pyrolysis carbon black dry granulation method. Compared with the prior art, the present invention has the following beneficial effects:

[0028] The dry granulation device and granulation method of the present invention can reprocess the pyrolysis carbon black of poor quality, reduce the particle size of the pyrolysis carbon black, and improve the reinforcement effect of the pyrolysis carbon black. At the same time, the reinforcing and dispersing performance of the pyrolysis carbon black is improved by adding a modifier. The oil content that affects the performance of the pyrolysis carbon black is reduced by high-temperature dry granulation, which is equivalent to secondary pyrolysis, thereby improving the quality of the pyrolysis carbon black and further improving the performance of the pyrolysis carbon black.

[0029] The pyrolysis carbon black dry granulation device and granulation method of the present invention solve the problem that the conventional carbon black dry granulation cannot granulate the pyrolysis carbon black, that is, a low-cost pyrolysis carbon black granulation method is provided, and the quality of the pyrolysis carbon black can be improved through the granulation process;

[0030] The pyrolysis carbon black particles obtained by the dry granulation device and granulation method of the present invention have excellent performance and a high degree of synthesis in the processing technology, and solve the problem of high round-trip transportation and storage costs caused by the step-by-step processing of first production, then modification, and then granulation in the existing pyrolysis carbon black production process. The present invention can continuously modify and process the pyrolysis carbon black, and has high processing efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0032] Figure 1 It is a structural schematic diagram of a dry granulation device according to an embodiment of the present invention;

[0033] Figure 2 It is a schematic structural diagram of a degassing device according to an embodiment of the present invention;

[0034] Figure 3 is a schematic diagram of a feed bin according to an embodiment of the present invention;

[0035] Figure 4 is a schematic diagram of a grinding and modification device according to an embodiment of the present invention;

[0036] Figure 5 Schematic diagram of a heating box according to an embodiment of the present invention.

[0037] In the figure:

[0038] 100 - feed bin, 110 - bin body, 120 - first heat-conducting layer, 130 - heating rod, 200 - degassing device, 210 - degassing pipeline, 211 - auger, 212 - filter element, 220 - vacuum pipeline, 230 - vacuum pump, 300 - tablet pressing device, 310 - pressure roller, 320 - conductive slip ring, 400 - shaping machine, 410 - crusher, 420 - screening machine, 500 - balanced distributor, 510 - second heat-conducting layer, 600 - heating box, 700 - grinding and modification equipment. DETAILED DESCRIPTION

[0039] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0040] like Figure 1 As shown, an embodiment of the present invention provides a dry granulation device, including a feed bin 100, a degassing device 200, a tablet pressing device 300 and a shaping machine 400;

[0041] The feed bin 100 is provided with a heating component for receiving and heating the raw material; the degassing device 200 is connected to the feed bin 100 and is used for degassing the heated raw material;

[0042] The tablet pressing device 300 is connected to the degassing device 200 and is arranged at the bottom of the degassing device 200 to tablet the degassed raw material; the shaping machine 400 is located at the bottom of the tablet pressing device 300 and is used to crush the tableted raw material into particles.

[0043] When the dry granulation device of the present invention is applied to the dry granulation of cracked carbon black, the heating function of the feed bin 100 is not only beneficial to the granulation of cracked carbon black, but also the oil contained therein will volatilize in large quantities through high temperature, thereby achieving the purpose of reducing the oil content in the cracked carbon black; the degassing device 200 can effectively increase the light and heavy density of the powdered carbon black, improve the granulation effect, and discharge the impurities, solvents and other small molecular substances adsorbed on the surface of the cracked carbon black after high-temperature volatilization.

[0044] like Figure 3 As shown, in some embodiments of the present invention, the feed bin 100 includes a bin body 110 and a first heat-conducting layer 120; the bin body 110 is used to receive raw materials, and the first heat-conducting layer 120 is arranged around the periphery of the bin body 110, and the first heat-conducting layer 120 is filled with a heat-conducting medium, which can be heat-conducting oil, for heating the raw materials.

[0045] Furthermore, a heating rod 130 may be provided in the silo body 110. Since the heat-conducting medium is coated on the outside of the silo body 110, when the amount of raw material fed is large, a large temperature difference may occur between the part inside the silo and the part close to the first heat-conducting layer 120. At this time, the raw material inside the silo may be heated by the heating rod 130 to keep the raw material in the silo evenly heated.

[0046] Furthermore, the silo body 110 can be set to a straight cylindrical shape or a funnel shape, preferably a funnel shape, which can not only increase the volume of the silo body 110, but also speed up the unloading speed and avoid blockage; and the unloading speed of the feed silo 100 is controlled and adjusted by an automatic butterfly valve.

[0047] like Figure 2 As shown, in some embodiments of the present invention, the degassing device 200 includes a degassing pipeline 210, a vacuum pipeline 220 and a vacuum pump 230; wherein the degassing pipeline 210 is arranged at the bottom of the feed bin 100, and an auger 211 is arranged in the degassing pipeline 210 for conveying raw materials; and a filter element 212 is arranged in the degassing pipeline 210 for filtering out impurities in the raw materials; the vacuum pipeline 220 is connected to the degassing pipeline 210; the vacuum pump 230 is connected to the vacuum pipeline 220, and the vacuum pressure is transmitted to the degassing pipeline 210 through the vacuum pump 230 and the vacuum pipeline 220 to remove small molecules such as impurities and solvents adsorbed on the surface of the cracked carbon black.

[0048] In some embodiments of the present invention, the tableting device 300 includes a pressing roller 310, a heating rod 130 and a conductive slip ring 320; wherein the pressing roller 310 is located at the bottom of the degassing pipeline 210, and is used to perform tableting operations on the raw materials; the heating rod 130 runs through the inside of the pressing roller 310 to heat the pressing roller 310, and performs high-temperature treatment on the raw materials during the tableting process, thereby effectively improving the dispersion of the raw materials; the conductive slip ring 320 is sleeved on the end of the rotating shaft of the pressing roller 310, and is used to provide power for the transmission equipment and the heating equipment.

[0049] In some embodiments of the present invention, the shaping machine 400 includes a crusher 410 and a screening machine 420; wherein the crusher 410 is located at the bottom of the pressure roller 310 device, and is used to crush the raw materials after tableting into particles; the screening machine 420 is connected to the bottom of the crusher 410, and is used to screen the crushed particles, and the qualified particles are transported to the qualified product storage tank through a belt, and the unqualified particles are recovered to the feed bin 100 for recycling treatment.

[0050] Specifically, when the dry granulation device is applied to pyrolysis carbon black, the function of the shaping machine 400 is to evenly crush the pyrolysis carbon black after tableting into particles, and after screening by the screening machine 420, the particle hardness is between 30-80, and the unqualified pyrolysis carbon black is recovered and re-participated in granulation.

[0051] In some embodiments of the present invention, a material balanced distributor 500 is further included, which is disposed between the feed bin 100 and the degassing device 200 and is used to mix the incoming raw materials and the recycled particles; further, a second heat-conducting layer 510 is disposed on one side of the material balanced distributor 500, and a heat-conducting medium is disposed in the second heat-conducting layer 510, and the heat-conducting medium is preferably heat-conducting oil, so as to properly keep the raw materials warm and reduce the cooling rate of the raw materials;

[0052] 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. Figure 5As shown, a heating rod 130 is provided in the heating box 600 to realize the recycling of the heat-conducting medium, and when the heat-conducting medium of the first heat-conducting layer 120 and the second heat-conducting layer 510 is the same, the two can share a 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 connected to 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 connected to the oil inlets of the first heat-conducting layer 120 and the second heat-conducting layer 510, to form a circulation loop, thereby realizing the recycling of the heat-conducting medium.

[0053] like Figure 4 As shown, in some embodiments of the present invention, a grinding and modification device 700 is also included, which is connected to the feed port of the feed bin 100. When the raw materials need to be modified, the raw materials are first modified by the grinding and modification device 700 and ground to a certain particle size and then transported to the feed bin 100 for subsequent processing.

[0054] The dry granulation device of the present invention can continuously modify and subsequently process raw materials without incurring high transportation and storage costs, thereby improving the processing efficiency while improving the performance of the raw materials, and is suitable for industrial production.

[0055] In addition, in some other embodiments of the present invention, a method for dry granulation of pyrolysis carbon black using any of the above-mentioned devices is provided, comprising the following steps:

[0056] Step S100. Pyrolysis carbon black modification: adding a modifier to the pyrolysis carbon black, grinding and mixing, and obtaining modified pyrolysis carbon black;

[0057] In the embodiment of the present invention, a modifier is added to improve the reinforcing and dispersing performance of the pyrolysis carbon black, wherein the amount of the modifier added is 1-15% of the mass of the pyrolysis carbon black, preferably 1-10%, more preferably 2-8%, for example, 2%, 5%, 8%, etc.;

[0058] Furthermore, the modifier includes a reinforcing tackifying resin, a carbon black coupling agent and a carbon black dispersant in a mass ratio of 2: (0.01-0.5): (0.01-0.5); wherein the carbon black coupling agent includes but is not limited to a silane coupling agent and a titanate coupling agent, and the carbon black dispersant includes but is not limited to styrene-butadiene-styrene copolymer (SBS), polymethyl methacrylate (PMMA), and polyvinyl alcohol (PVA), which are mainly used to improve the dispersion performance of cracked carbon black, avoid agglomeration in the subsequent rubber preparation process, and improve mechanical properties such as strength, hardness, and wear resistance; and the mass ratio of the reinforcing tackifying resin, the carbon black coupling agent and the carbon black dispersant 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 can be adjusted within this range according to actual conditions.

[0059] Furthermore, the reinforcing and tackifying resin includes a reinforcing resin and a tackifying resin in a mass ratio of (0.01-2):(0.01-5), and the mass ratio of the reinforcing resin and the tackifying resin can be 1:1, 2:0.01, 0.01:2, 0.05:5, etc., which is used to improve the reinforcing performance of the pyrolysis carbon black and improve the quality of the pyrolysis carbon black.

[0060] Furthermore, the grinding in step (1) is carried out in a ball mill, and the material-ball ratio of the mill is 1:1-3, the ball milling speed is 30-50 Hz / min, and the ball milling time is 10-50 min. Controlling the appropriate material-ball ratio, ball milling speed and ball milling time can improve the dispersion performance of the pyrolysis carbon black to a certain extent.

[0061] Step S200. The modified pyrolysis carbon black is transported to the feed bin 100 for heating and deoiling treatment, and then enters the degassing device 200 for degassing treatment. The degassed pyrolysis carbon black is tableted at high temperature by the tableting device 300, and then continues to be crushed, granulated and screened by the shaping machine 400.

[0062] This step can effectively reduce the oil content in the pyrolysis carbon black through high-temperature dry granulation, which is equivalent to a secondary pyrolysis process and can further improve the quality and performance of the pyrolysis carbon black.

[0063] Furthermore, in step (2), the feed rate of the modified pyrolysis carbon black to the feed bin 100 is 100-800 kg / h, preferably 150-600 kg / h, more preferably 200-500 kg / h, for example, 200 kg / h, 350 kg / h, 500 kg / h, etc., which can keep the dry granulation process going and reduce the transportation and storage costs. Maintaining the feed rate can ensure that the impurities in the subsequent degassing process are removed more completely and the tablet thickness is moderate.

[0064] Furthermore, the heating and deoiling temperature of the feed bin 100 is 150-400°C, for example, 150°C, 300°C, 400°C, etc., and the oily substance coated on the surface of the pyrolysis carbon black is removed by high-temperature heating treatment to improve the dispersibility of the pyrolysis carbon black.

[0065] Furthermore, during the degassing process, the vacuum pressure of the degassing device 200 is 0.1-1.0 MPa, for example, it can be 0.1 MPa, 0.5 MPa, 1.0 MPa, etc. The degassing process can remove impurities and solvents on the surface of the pyrolysis carbon black to improve the purity of the product. In addition, the dry granulation device can be placed in a negative pressure environment by vacuuming to obtain pyrolysis carbon black of suitable particle size and enhance the dispersion performance.

[0066] Furthermore, the high-temperature tableting temperature of the tableting device 300 is 150-400°C, for example, 150°C, 300°C, 400°C, etc., so that the pyrolysis carbon black is continuously kept at a high temperature during the dry granulation process, thereby improving the granulation effect of the pyrolysis carbon black, as well as improving the reinforcement and dispersion properties of the pyrolysis carbon black.

[0067] The dry granulation process of pyrolysis carbon black of the present invention is described in detail below with reference to specific embodiments.

[0068] Example 1

[0069] This embodiment provides a method for dry granulation of pyrolysis carbon black, comprising the following steps:

[0070] (1) The pyrolysis carbon black is subjected to ultrafine grinding by air milling, and the power of the main grinding machine is 50 Hz;

[0071] (2) adding 8% of a modifier to the pyrolysis carbon black, mixing the pyrolysis carbon black with the modifier in a cone mixer, and then grinding and mixing the pyrolysis carbon black in a grinder at a ball milling speed of 30 Hz / min for 20 minutes, so that the modifier and the pyrolysis carbon black undergo a grafting reaction during the grinding process to obtain modified pyrolysis carbon black; wherein the modifier comprises a reinforcing tackifying resin, a silane coupling agent KH-550 and a styrene-butadiene-styrene copolymer in a mass ratio of 2:0.3:0.05; the reinforcing tackifying resin comprises a tall oil-modified phenolic reinforcing resin and an octylphenolic tackifying resin in a mass ratio of 1:1, and the material-to-ball ratio of the grinder is 1:1-3;

[0072] (3) The modified pyrolysis carbon black is added to the dry granulation device, and the feed rate is controlled to be 450 kg / h. After the pyrolysis carbon black is transported to the feed bin, it is treated at 250° C. and then enters the degassing device. The vacuum pump pressure of the degassing device is set to 0.6 MPa. The degassed pyrolysis carbon black enters the pressing roller and is pressed into sheets at a high temperature of 250° C. The motor speed of the pressing roller is 50 Hz. The sheeted pyrolysis carbon black enters the shaping machine, and the pressed pyrolysis carbon black is evenly crushed into particles. Qualified particles with a hardness of 40-70 are screened and unqualified particles are recovered to the feed bin for re-granulation.

[0073] Example 2

[0074] This embodiment provides a method for dry granulation of pyrolysis carbon black, comprising the following steps:

[0075] (1) The pyrolysis carbon black is subjected to ultrafine grinding by air milling, and the power of the main grinding machine is 20 Hz;

[0076] (2) adding 3% of a modifier to the pyrolysis carbon black, mixing the pyrolysis carbon black with the modifier in a cone mixer, and then grinding and mixing the pyrolysis carbon black in a grinder at a ball milling speed of 40 Hz / min for 30 minutes, so that the modifier and the pyrolysis carbon black undergo a grafting reaction during the grinding process to obtain modified pyrolysis carbon black; wherein the modifier comprises a reinforcing tackifying resin, a silane coupling agent KH-560 and polymethyl methacrylate in a mass ratio of 2:0.01:0.5; the reinforcing tackifying resin comprises a tall oil modified phenolic reinforcing resin and a colloxane tackifying resin in a mass ratio of 0.01:5, and the material-to-ball ratio of the grinder is 1:1-3;

[0077] (3) The modified pyrolysis carbon black is added to the dry granulation device, and the feed rate is controlled to be 600 kg / h. After the pyrolysis carbon black is transported to the feed bin, it is treated at 150° C. and then enters the degassing device. The vacuum pump pressure of the degassing device is set to 0.3 MPa. The degassed pyrolysis carbon black enters the pressing roller and is pressed into sheets at a high temperature of 150° C. The motor speed of the pressing roller is 10 Hz. The sheeted pyrolysis carbon black enters the shaping machine, and the pressed pyrolysis carbon black is evenly crushed into particles. Qualified particles with a hardness of 40-70 are screened and unqualified particles are recovered to the feed bin for re-granulation.

[0078] Example 3

[0079] This embodiment provides a method for dry granulation of pyrolysis carbon black, comprising the following steps:

[0080] (1) The pyrolysis carbon black is subjected to ultrafine grinding by air milling, and the power of the main grinding machine is 80 Hz;

[0081] (2) adding 1% of a modifier to the pyrolysis carbon black, mixing the pyrolysis carbon black with the modifier in a cone mixer, and then grinding and mixing the pyrolysis carbon black in a grinder at a ball milling speed of 50 Hz / min for 10 minutes, so that the modifier and the pyrolysis carbon black undergo a grafting reaction during the grinding process to obtain modified pyrolysis carbon black; wherein the modifier comprises a reinforcing tackifying resin, a silane coupling agent KH570 and polyvinyl alcohol in a mass ratio of 2:0.02:0.01; the reinforcing tackifying resin comprises a high styrene resin and a tert-butyl tackifying resin in a mass ratio of 2:0.01, and the material-to-ball ratio of the grinder is 1:1-3;

[0082] (3) The modified pyrolysis carbon black is added to the dry granulation device, and the feed rate is controlled to be 100 kg / h. After the pyrolysis carbon black is transported to the feed bin, it is treated at 300° C. and then enters the degassing device. The vacuum pump pressure of the degassing device is set to 1.0 MPa. The degassed pyrolysis carbon black enters the pressing roller and is pressed into sheets at a high temperature of 300° C. The motor speed of the pressing roller is 30 Hz. The sheeted pyrolysis carbon black enters the shaping machine, and the pressed pyrolysis carbon black is evenly crushed into particles. Qualified particles with a hardness of 40-70 are screened and unqualified particles are recovered to the feed bin for re-granulation.

[0083] Example 4

[0084] This embodiment provides a method for dry granulation of pyrolysis carbon black, comprising the following steps:

[0085] (1) The pyrolysis carbon black is subjected to ultrafine grinding by air milling, and the power of the main grinding machine is 100 Hz;

[0086] (2) adding 15% of a modifier to the pyrolysis carbon black, mixing the pyrolysis carbon black with the modifier in a cone mixer, and then grinding and mixing the pyrolysis carbon black in a grinder at a ball milling speed of 35 Hz / min for 50 minutes, so that the modifier and the pyrolysis carbon black undergo a grafting reaction during the grinding process to obtain modified pyrolysis carbon black; wherein the modifier comprises a reinforcing tackifying resin, a titanate coupling agent, and polyvinyl alcohol in a mass ratio of 2:0.4:0.09; the reinforcing tackifying resin comprises a high styrene resin and an octylphenol formaldehyde tackifying resin in a mass ratio of 0.5:3.2, and the material-to-ball ratio of the grinder is 1:1-3;

[0087] (3) The modified pyrolysis carbon black is added to the dry granulation device, and the feed rate is controlled to be 800 kg / h. After the pyrolysis carbon black is transported to the feed bin, it is treated at 400°C and then enters the degassing device. The vacuum pump pressure of the degassing device is set to 0.1 MPa. The degassed pyrolysis carbon black enters the pressing roller and is pressed into sheets at a high temperature of 400°C. The speed of the pressing roller motor is 60 Hz. The sheeted pyrolysis carbon black enters the shaping machine, and the pressed pyrolysis carbon black is evenly crushed into particles. Qualified particles with a hardness of 40-70 are screened and unqualified particles are recovered to the feed bin for re-granulation.

[0088] The pyrolysis carbon black particles of Example 1-4 are used to prepare vulcanized rubber, and the steps are as follows: the pyrolysis carbon black particles are mixed with natural rubber, stearic acid, zinc oxide, accelerator DM, and sulfur in a mass ratio of 50:100:3:5:0.6:2.5 for rubber refining, and vulcanizing at 145°C to obtain vulcanized rubber.

[0089] The physical properties of the pyrolysis carbon black particles obtained in Examples 1-4 and the physical properties of the vulcanized rubber prepared by pyrolysis carbon black particles in Examples 1-4 were measured. The results are shown in Table 1:

[0090] Table 1

[0091]

[0092] Comparative Example 1

[0093] This comparative example is basically the same as Example 1, the only difference being that 0.5% of a modifier is added in step (2).

[0094] Comparative Example 2

[0095] This comparative example is basically the same as Example 1, the only difference being that 16% of a modifier is added in step (2).

[0096] Comparative Example 3

[0097] This comparative example is basically the same as Example 1, the only difference being that 20% of a modifier is added in step (2).

[0098] The physical properties of the pyrolysis carbon black particles obtained in Comparative Examples 1-3 and the physical properties of the vulcanized rubber prepared by pyrolysis carbon black particles in Comparative Examples 1-3 were measured. The results are shown in Table 2:

[0099] Table 2

[0100]

[0101] As shown in Table 2, the addition of modifier can greatly improve the dispersibility and reinforcement performance of pyrolysis carbon black. After using the modifier, the tensile strength and 300% elongation stress performance of pyrolysis carbon black in rubber are improved. When the amount of modifier added is too little, the dispersibility and reinforcement performance of the modified pyrolysis carbon black are poor, and the ash value is high; when the amount added is too much, the performance of the modified pyrolysis carbon black and the rubber performance will not change significantly, and the ash value will increase. Therefore, the amount of modifier added is determined to be 1-15% of the mass of pyrolysis carbon black.

[0102] Comparative Example 4

[0103] This comparative example is basically the same as Example 1, except that the modifier in step (2) is a silane coupling agent KH-550 and a styrene-butadiene-styrene copolymer in a mass ratio of 0.3:0.05, and no reinforcing tackifying resin is added.

[0104] Comparative Example 5

[0105] This comparative example is basically the same as Example 1, except that the modifier in step (2) is a phenolic reinforcing resin modified with tall oil, a silane coupling agent KH-550 and a styrene-butadiene-styrene copolymer in a mass ratio of 2:0.3:0.05, and no tackifying resin is added.

[0106] Comparative Example 6

[0107] This comparative example is basically the same as Example 1, except that the modifier in step (2) is octylphenol formaldehyde tackifying resin, silane coupling agent KH-550 and styrene-butadiene-styrene copolymer in a mass ratio of 2:0.3:0.05, and no reinforcing resin is added.

[0108] Comparative Example 7

[0109] This comparative example is basically the same as Example 1, except that: in step (2), the modifier comprises a reinforcing tackifying resin, a silane coupling agent KH-550 and a styrene-butadiene-styrene copolymer in a mass ratio of 1:0.3:0.05; and the reinforcing tackifying resin comprises a tall oil-modified phenolic reinforcing resin and an octylphenolic tackifying resin in a mass ratio of 1:1.

[0110] The physical properties of the pyrolysis carbon black particles obtained in Comparative Examples 4-7 and the physical properties of the vulcanized rubber prepared from the pyrolysis carbon black particles in Comparative Examples 4-7 were measured. The results are shown in Table 3:

[0111] Table 3

[0112]

[0113] As shown in Table 3, the modifier can greatly improve the dispersibility and reinforcement properties of the modified pyrolysis carbon black, and the tensile strength and 300% modulus stress of the pyrolysis carbon black in the rubber are improved after using the modifier. When the type of modifier or the proportion of the modifier changes, it will have a greater impact on the mechanical properties of the vulcanized rubber.

[0114] Comparative Example 8

[0115] This comparative example is basically the same as Example 1, with the only difference being that in step (3), the feed rate of the modified pyrolysis carbon black to the feed bin is 50 kg / h.

[0116] Comparative Example 9

[0117] This comparative example is basically the same as Example 1, with the only difference being that in step (3), the feed rate of the modified pyrolysis carbon black to the feed bin is 900 kg / h.

[0118] Comparative Example 10

[0119] This comparative example is basically the same as Example 1, with the only difference being that in step (3), the feed rate of the modified pyrolysis carbon black to the feed bin is 1000 kg / h.

[0120] The physical properties of the pyrolysis carbon black particles obtained in Comparative Examples 8-10 and the physical properties of the vulcanized rubber prepared by pyrolysis carbon black particles in Comparative Examples 8-10 were measured. The results are shown in Table 4:

[0121] Table 4

[0122]

[0123] It can be seen from Table 4 that the feeding speed mainly affects the particle quality of the cracked carbon black after modified granulation. If the feeding speed is low, the particles will be unevenly granulated, the crushing strength will be low, and the fine powder content will be too high. If the feeding speed is high, it will not have a significant change on the particle performance, but it will increase energy consumption. Therefore, the feeding speed is limited to 100-800kg / h based on comprehensive considerations.

[0124] Comparative Example 11

[0125] This comparative example is basically the same as Example 1, with the only difference being that the pyrolysis carbon black is treated at room temperature after being transported to the feed bin.

[0126] Comparative Example 12

[0127] This comparative example is basically the same as Example 1, with the only difference being that the pyrolysis carbon black is treated at 100° C. after being transported to the feed bin.

[0128] Comparative Example 13

[0129] This comparative example is basically the same as Example 1, with the only difference being that the pyrolysis carbon black is treated at 450° C. after being transported to the feed bin.

[0130] Comparative Example 14

[0131] This comparative example is basically the same as Example 1, with the only difference being that the pyrolysis carbon black is treated at 550° C. after being transported to the feed bin.

[0132] The physical properties of the pyrolysis carbon black particles obtained in Comparative Examples 11-14 and the physical properties of the vulcanized rubber prepared by pyrolysis carbon black particles in Comparative Examples 11-14 were measured. The results are shown in Table 5:

[0133] Table 5

[0134]

[0135]

[0136] It can be seen from Table 5 that heating deoiling can effectively improve the granulation quality and the reinforcement effect of the modified pyrolysis carbon black, the particle crushing strength distribution is more uniform, and the tensile strength and tensile stress of the vulcanized rubber prepared therefrom are improved.

[0137] Comparative Example 15

[0138] This comparative example is basically the same as Example 1, with the only difference being that in step (3), the modified pyrolysis carbon black is not subjected to degassing treatment.

[0139] Comparative Example 16

[0140] This comparative example is basically the same as Example 1, with the only difference being that the vacuum pressure of the degassing device during the degassing process is 1.2 MPa.

[0141] Comparative Example 17

[0142] This comparative example is basically the same as Example 1, with the only difference being that the vacuum pressure of the degassing device during the degassing process is 1.5 MPa.

[0143] The physical properties of the pyrolysis carbon black particles obtained in Comparative Examples 15-17 and the physical properties of the vulcanized rubber prepared from the pyrolysis carbon black particles in Comparative Examples 15-17 were measured. The results are shown in Table 6:

[0144] Table 6

[0145]

[0146]

[0147] As shown in Table 6, vacuum degassing can effectively discharge high-temperature volatile substances, reduce the ash content of pyrolysis carbon black, and improve the tensile strength and 300% elongation stress of vulcanized rubber. After research, it was found that without vacuum degassing, even with heating and deoiling treatment, it is difficult to effectively granulate, and the pyrolysis carbon black granulation yield is low, only 40-60%; after heating and deoiling and vacuum degassing treatment, the ash content can be effectively reduced and the mechanical properties of vulcanized rubber can be enhanced; because when the vacuum degassing pressure exceeds 1MPa, its various properties will not be significantly improved, so the vacuum degassing pressure is limited to 0.1-1MPa.

[0148] Comparative Example 18

[0149] This comparative example is substantially the same as Example 1, the only difference being that tableting is performed at room temperature.

[0150] Comparative Example 19

[0151] This comparative example is substantially the same as Example 1, except that the high temperature tableting temperature is 100°C.

[0152] Comparative Example 20

[0153] This comparative example is basically the same as Example 1, the only difference being that the high-temperature tableting temperature is 450°C.

[0154] The physical properties of the pyrolysis carbon black particles obtained in Comparative Examples 18-20 and the physical properties of the vulcanized rubber prepared by pyrolysis carbon black particles in Comparative Examples 18-20 were measured. The results are shown in Table 7:

[0155] Table 7

[0156]

[0157]

[0158] It can be seen from Table 6 that the higher the tableting temperature, the better the performance of the modified pyrolysis carbon black and the performance of the vulcanized rubber. However, when the tableting temperature reaches a certain value, the performance improvement is not significant. Considering the energy consumption comprehensively, the tableting temperature is limited to 150-400°C. It is found through research that compared with tableting at room temperature, tableting under heating conditions can effectively improve the granulation effect of pyrolysis carbon black, and the particle shape is more uniform and the dispersion is better.

[0159] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the scheme disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0160] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for dry granulation of pyrolysis carbon black, characterized in that: The following steps are involved: (1) Pyrolysis carbon black modification: adding a modifier to the pyrolysis carbon black, grinding and mixing, and obtaining modified pyrolysis carbon black; (2) The modified pyrolysis carbon black is transported to the feed bin for heating and de-oiling treatment, and then enters the degassing device for degassing treatment. The degassed pyrolysis carbon black is tableted at high temperature in the tableting device, and then continues to be crushed, granulated and screened in the shaping machine; The amount of the modifier added in step (1) is 1-15% of the mass of the pyrolysis carbon black; and / or the modifier comprises a reinforcing tackifying resin, a carbon black coupling agent and a carbon black dispersant in a mass ratio of 2:(0.01-0.5):(0.01-0.5); and / or the reinforcing and tackifying resin comprises a reinforcing resin and a tackifying resin in a mass ratio of (0.01-2):(0.01-5); The grinding in step (1) is carried out in a ball mill, with a material-to-ball ratio of 1:1-3, a ball milling speed of 30-50 Hz / min, and a ball milling time of 10-50 min; The modified pyrolysis carbon black in step (2) is transported to the feed bin at a rate of 100-800 kg / h; and / or the heating and deoiling temperature of the feed bin is 150-400°C; And / or the vacuum pressure of the degassing device during the degassing process is 0.1-1.0MPa; And / or the high temperature tableting temperature of the tableting device is 150-400°C.

2. A method for dry granulation of pyrolysis carbon black according to claim 1, characterized in that: The dry granulation device used includes: A feed bin, wherein a heating component is provided in the feed bin for receiving and heating the raw materials; A degassing device, connected to the feed bin, for degassing the heated raw material; A tableting device, connected to the degassing device and arranged at the bottom of the degassing device, to tablet the degassed raw material; The shaping machine is located at the bottom of the tablet pressing device and is used to crush the tabletted raw materials into particles.

3. A method for dry granulation of pyrolysis carbon black according to claim 2, characterized in that: The feed bin comprises: A silo body, used for receiving raw materials; The first heat-conducting layer is arranged around the periphery of the chamber body, and the first heat-conducting layer is filled with a heat-conducting medium.

4. A method for dry granulation of pyrolysis carbon black according to claim 2, characterized in that: The degassing device comprises: A degassing pipeline is arranged at the bottom of the feed bin, and an auger is arranged in the degassing pipeline for conveying raw materials; and a filter element is arranged in the degassing pipeline for filtering out impurities in the raw materials; A vacuum pipeline connected to the degassing pipeline; A vacuum pump is connected to the vacuum pumping pipeline, and the vacuum pressure is transmitted to the degassing pipeline through the vacuum pump and the vacuum pumping pipeline.

5. A method for dry granulation of pyrolysis carbon black according to claim 4, characterized in that: The tablet pressing device comprises: A pressing roller, located at the bottom of the degassing pipeline, used for tableting the raw materials; A heating rod, which runs through the interior of the pressing roller to heat the pressing roller; The conductive slip ring is sleeved on the end of the rotating shaft of the pressing roller.

6. A method for dry granulation of pyrolysis carbon black according to claim 5, characterized in that: The shaping machine comprises A crusher, located at the bottom of the pressing roller device, is used to crush the raw materials after tableting into particles; The screening machine is connected to the bottom of the crusher and is used to screen the crushed particles. The qualified particles are conveyed to the qualified product storage tank through a belt, and the unqualified particles are recovered to the feed bin for recycling.

7. A method for dry granulation of pyrolysis carbon black according to claim 3, characterized in that: It also includes a material balance distributor, which is arranged between the feed bin and the degassing device and is used to mix the new raw materials and the recycled particles; And / or a second heat-conducting layer is provided on one side of the material balanced distributor, and a heat-conducting medium is provided in the second heat-conducting layer; And / or the first heat-conducting layer and the second heat-conducting layer are both connected to a heating box to achieve recycling of the heat-conducting medium.

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