WO2018122017A1 - Procédé de préparation de noir de carbone et procédé de fabrication d'un prémélange pour une installation de mélange de caoutchouc - Google Patents

Procédé de préparation de noir de carbone et procédé de fabrication d'un prémélange pour une installation de mélange de caoutchouc Download PDF

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Publication number
WO2018122017A1
WO2018122017A1 PCT/EP2017/083239 EP2017083239W WO2018122017A1 WO 2018122017 A1 WO2018122017 A1 WO 2018122017A1 EP 2017083239 W EP2017083239 W EP 2017083239W WO 2018122017 A1 WO2018122017 A1 WO 2018122017A1
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WIPO (PCT)
Prior art keywords
carbon black
steam
stage
grinding
compound
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Application number
PCT/EP2017/083239
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German (de)
English (en)
Inventor
Guido Veit
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Zeppelin Systems Gmbh
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Publication of WO2018122017A1 publication Critical patent/WO2018122017A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C09C1/58—Agglomerating, pelleting, or the like by wet methods
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/482—Preparation from used rubber products, e.g. tyres
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C09C1/60—Agglomerating, pelleting, or the like by dry methods

Definitions

  • the invention relates to a process for the preparation of carbon black (CB), in particular recycled carbon black (rCB) and a production process for the preparation of a pre-compound.
  • CB carbon black
  • rCB recycled carbon black
  • Rubber manufacturers usually use perlusses in large quantities as additives in rubber production. In the rubber mixing process, numerous other additives are added to the mixture. Usually, the recipe is prepared individually for each approach from the raw materials.
  • soot represents a separate, investment-intensive and energy-intensive process stage.
  • the batching is mainly carried out in order to make soot manageable for the distribution process. Nevertheless, this handling is not without problems. Improper handling greatly limits the usefulness of the soot or leads, for example, to severe pollution of the environment.
  • the method described here could also be adapted to production processes of technical Russian according to conventional production methods. In the following, however, is initially on the treatment of CB from a pyrolytic Recycling plant for rubber products, especially tires are received.
  • binders are added to the water or beading is improved by the addition of "seed” or wax, but these binder aids or beading aids remain in the carbon black.
  • EP 0 924 268 B1 discloses a process for producing pearlite in which the present-day common process is well described and consists in principle of the sequence of a grinding step, a filtration step, a batching step and a drying step.
  • the starting point of the drying step is thus a pelleted carbon black (CB).
  • a small filling quantity and a high fines content of the CB in the mixer have a disadvantageous effect on the mixing efficiency or the mixing quality or the achievable mixing throughput per time.
  • the invention is therefore based on the object, a method for the treatment of recycled carbon black (rCB) and a preparation of a pre-compound (PCO) for a rubber compounding educate such that at lower energy consumption, a higher production performance is ensured in the production of a rubber compound.
  • the advantage of the method according to the invention is that the elaborate batching and drying process is eliminated and thus an improved production can be achieved by the measures according to the invention.
  • PCO pre-compound
  • the further advantage of the invention is that based on the production of a pre-compound for a rubber mixing a higher degree of filling for the mixer and thus an increase in performance for the mixer can be achieved.
  • the degree of dispersion of the additives in the mixer can be improved, which was previously not possible in the prior art.
  • This can be countered by the fact that in industrial use, on the one hand, it can be expected that different pre-compounds with different compositions will be offered.
  • the required amount to be supplied per mixture becomes various recipe ingredients reduced, whereby these dosing are relieved or possibly bottlenecks can be eliminated.
  • these second carbon black base particles are mixed into a particle stream of the first carbon black base particles and subsequently a pelletization of the first and second carbon black base particles to form hybrid carbon black particles.
  • the mixing ratio between the new product soot and the recycled soot is fixed by the admixture of the second carbon black particles and can not be changed in the subsequent product.
  • the real disadvantage is also that virgin material is mixed with recycled goods, and thus the type and composition of the carbon black produced therewith is adversely determined from the outset.
  • the invention it is now proposed to use a pre-compound, which is produced via a specific process. The mixture is formed during the condensation and is qualified in an extrusion stage to a manageable commodity.
  • the use of recycled carbon black is favored. Condensation directly from the gas phase without a filter stage after dry-grinding with steam is novel, as is quenching with additives instead of water.
  • a new process path is proposed for refining carbon black and converting it into a tradable (logistically convertible commodity).
  • the invention can make the rubber manufacturing process more efficient by over 10%. It offers an economic trade route and new market access for recycled carbon black.
  • the present invention provides the following partial inventions, each of which should enjoy protection for each other individually but also in any combination:
  • the invention comprises several steps whose individual steps should enjoy protection both alone and in any combination with one another.
  • the previous investment-intensive filter stage can be significantly reduced.
  • this energy-intensive treatment process can be energetically optimized significantly.
  • a third step the condensation of water vapor is supported by quenching with additives.
  • a new form is created as a commercial product.
  • a pre-compound is to be produced, which can be handled much easier than pearl tufts and also shows many other advantages.
  • Part 1 - Elimination of the filter level The purpose of the invention is to eliminate the filter stage or replace it with a smaller filter elsewhere. This can significantly reduce the cost of grinding.
  • the grinding is carried out with the highest possible proportion of superheated steam instead of air (supercritical steam at a pressure level of about 30 to 40 bar).
  • the vapor-particle mixture is not passed through a filter, but via a cooling stage, which can condense the vapor. This exploits the fact that water vapor has a volume about 1,600 times that of water. The then condensed water is needed anyway in the downstream Verperlungswork. The heat of condensation is used to generate new steam.
  • Carbon black (CB) according to a pyrolytic process is usually cooled after the main process to below 40 ° C - 60 ° C for intermediate storage. For this purpose, usually cooling screws are used.
  • a disadvantage here is that in the unintentional whereabouts of small amounts of monomers and oil vapors in the recyclate an inflammable atmosphere can arise and thus limited storage life of recycled granules.
  • the invention is now to make this cooling with water, which is brought directly into contact with the recyclate.
  • the resulting water vapor is used in the downstream steam jet mill.
  • the recyclate is not cooled down to less than 130 ° C and immediately fed to the milling process to prevent premature condensation of the water vapor and the associated loss of performance.
  • the "extinguishing" of the recyclate with water has the further advantage that an inert atmosphere of water vapor significantly reduces the risk of spontaneous combustion.When only a limited expansion space is made available to the recycled-steam mixture, the evaporation of the water results in pressure build-up , which can be used advantageously for the operation of a steam jet mill, thereby significantly improving the energy balance.
  • the pyrolysis product is not cooled after pyrolysis, but fed directly hot steam jet mill.
  • an injector is used to accelerate the feed to the steam jet mill. This is operated with wet steam. The free water will evaporate on contact with the hot recyclate, resulting in dry steam of much greater volume. Since the vapor-particle mixture in the tube can not expand, there is a pressure and as a result to an increase in speed in the tube. This acts as a "booster" or "turbo" for the downstream grinding process.
  • the pyrolysis product is not cooled after pyrolysis, but fed directly hot steam jet mill.
  • To build up pressure before conveying the recyclate is collected in a pressure vessel and this is mixed with water. The free water will evaporate on contact with the hot recyclate, resulting in dry steam of much greater volume. Since the vapor-particle mixture in the pressure vessel can not expand, there is an increase in pressure in the pressure vessel. This acts as a "booster" or "turbo" for the downstream promotion to the grinding process.
  • the recycling CB is in the steam jet mill to particles between 2 ⁇ and 10 ⁇ milled.
  • the particle vapor stream from the steam jet mill is fed in a preferred embodiment, first in a stage for precooling.
  • the vapor-particle mixture is preferably cooled to the condensation point of the vapor.
  • the condensation point of the vapor is influenced, inter alia, by the pressure level of the vapor-particle mixture.
  • the mass flow emerging from the steam jet mill is completely supplied to the condensation. It is advantageous that can be completely dispensed with a complex and service-intensive filter stage.
  • a partial flow of the steam can be separated from the total mass flow via a filter and fed back to the steam jet mill via a treatment process.
  • the amount of additives required for complete condensation of the water vapor is reduced, thereby increasing the proportion of CB in the end product.
  • the gas stream to the gas jet mill can also be passed through a gas cyclone, in which case the gas stream with the coarse particles is returned to the gas jet mill and the gas stream is passed with the fine particles to condensation.
  • the fineness of the Aufmahlung or the product quality can be influenced.
  • the additives can positively influence the formation of the beads (condensation nuclei) or the strength of the beads.
  • Part 4 - Production of a Pre-Compound The additives are added to a far greater extent than would be required for the normal carbonization process of the carbon black.
  • silica can be used as additive and coolant.
  • Silica is increasingly used in many rubber compounds. Silica is just as difficult to handle as soot due to its low bulk density and the problem of bumping. Its low bulk density additionally causes difficulties in storage, metering and weighing as well as the degree of filling of the rubber mixer.
  • the limited volume of the mixing chamber limits the amount of silica that can be added to a mixture for a comparable amount of time.
  • the incorporation of silica in the current way greatly increases the wear in the mixer.
  • the use of pre-compound increases the degree of filling and reduces wear in the mixer.
  • the cooling provided by the introduced substances leads to a sudden cooling of the total material flow, which results in the spontaneous condensation of the water vapor and reduction in the volume of the vapor mixture.
  • the incorporated materials may be powdered, granular, liquid, solid, frozen, or any other state, and are preferably added at ambient or chilled. It is advantageous to supply these substances as small as possible particles so that the heat balance with the mixture can be achieved as quickly as possible.
  • a partial stream of the already condensed slurry can be separated off and recycled in cooled form instead of other additives to the wet steam mixture in order to assist the condensation.
  • the slurry can also be recycled in frozen form or added to the main stream. The cooling is thus particularly intensive, since the frozen slurry in addition to the specific heating heat until the mixture temperature, the heat of fusion extracts the multi-component mixture.
  • the pressure of the vapor mixture must be carefully observed and regulated or kept at a certain pressure level.
  • the shift of the condensation temperature with changing pressure must also be considered. This effect can be advantageously used to guide the condensation site.
  • quenching with water is used according to the known method, since it is inert on the composition of the formulation and water is already part of the mixture at this time of the process, but again before the product is finished almost completely removed ⁇
  • the substances introduced are anyway part of the recipe for which the pre-compound produced in this way is later used.
  • the mixture of substances produced in this way is a pre-compound which, due to its composition, can be incorporated into a multiplicity of common formulations by supplementing other substances or quantitatively supplementing the substances already present.
  • the mixture of substances produced in this way is a pre-compound which, after degassing the excess water by its composition, can assume a stable granular form which satisfies the logistical requirements.
  • the extruder instead of the granulation optimizes the mixing of the different feedstocks.
  • the addition of further additives is conceivable and intended.
  • the invention means a machine with one or more, rotating in a channel, screw-like spindles with patch mixing elements of various designs.
  • extruders are known in the machine design as extruders, compounders, co-rotors, counter-rotors, planetary roller extruders, ring extruders or kneaders and are used here.
  • the handling of pre-compound is easier than pearl pearl or
  • the pre-compound produced already represents an intimate mixture of various additives in a recipe. This reduces the mixing energy for the actual mixing process and increases the quality of the mixture with the same energy input.
  • the mixer e.g., an internal mixer for rubber in batch mode
  • the mixer can be given a higher mass with limited mixing chamber volume. This increases the specific throughput of the mixer and thus the efficiency of the entire mixer line.
  • superheated steam is used instead of air or combustion gases as a carrier medium for grinding.
  • the gas / soot particle mixture is treated via a process to steam just above the saturated steam region with a weight fraction of soot particles preferably between 0.1 and 50 wt .-%.
  • the bandwidth varies greatly and is strongly influenced by the grinding properties and in particular the desired Aufmahlungsgrad or the desired to be achieved average grain size of the ground product.
  • the proportion of different configurations of gas cyclone and / or filters can be favorably influenced.
  • the recycled soot is milled to a mean particle size of between 1 and 6 ⁇ m and concentrated to a weight fraction of from 7 to 30% by weight of carbon black via a gas cyclone and a subsequent filter stage.
  • This vapor / substance mixture is "quenched" (quenching) by adding additives that are cooler than the vapor / substance mixture, and this results in spontaneous and rapid condensation of the vapor, which increases the volume of the vapor. / Substance mixture reduced by the factor> 1000.
  • the added additives are anyway components of the formulations of the further processing of the product.
  • the multicomponent mixture thus obtained is optionally supplied with a high proportion of water to a batch in a beading machine or a granulation in an extruder. 7. In a granulation in an extruder other substances are added, the mass is mixed intensively and the heat of evaporation of the outgassing water significantly contributes to the cooling of the mix in the extruder.
  • the final composition of the precompound is determined by the addition of the additives. This is preferably chosen so that a stable granules with good properties in terms of storage, delivery and dosage arises.
  • Recycling CB produced in the process 50 of FIG. 6c has, according to experience, a certain fluctuation range in the composition, since this is determined by the starting materials and these are usually subject to fluctuations in a recycling process.
  • the extruder 17 supplied product see Figure 1.
  • the final composition of the precompound is determined by the addition of the additives.
  • the amount of added additives is preferably chosen so that volume fluctuations of individual components in the input branch 1 6 is compensated by adjusting the amount of additives added via the access branch 20 in such a way that the composition of the granules 28 is kept within the narrowest possible limits.
  • the gas stream is condensed according to the invention.
  • the condensed gas is then evaporated again from the solid.
  • a substance or more substances is injected (quench) in such an amount according to the invention, so that the mixing temperature of the resulting two- or multi-component mixture is below the condensation temperature of the carrier gas and the carrier gas condenses.
  • the invention therefore relates to a method for direct blasting of CB from a jet mill while avoiding the filter stage by condensation of the carrier gas.
  • the associated advantage is that water vapor is used as the carrier medium for the jet mill instead of air.
  • the steam can be condensed and does not have to be separated from the regrind, since the water is used anyway for the grinding of soot.
  • the rapid condensation of a large amount of steam requires the rapid removal of large amounts of heat. This represents a high outlay in terms of apparatus. This is achieved by "quenching" in the sense of the invention. 2.
  • Recycle Compound Compound The invention also relates to a process for preparing a masterbatch (pre-compound) from rCB in conjunction with e.g. Liquid Rubber, waxes or other additives. It is therefore proposed that the preparation of premixes of silica and CB in conjunction with liquids and waxes for ease of handling in the mixing process and increase the mixing throughput and the mixer efficiency is done.
  • the associated advantage is that premixes of silica or CB are easier to handle than the bulk materials alone.
  • the degree of filling of the mixer can be increased. Presumably, the dispersion is improved and the wear of the mixer is reduced.
  • the inventive idea also relates to the combination of recycled carbon black and filler compound in that a process for preparing a masterbatch (pre-compound) from rCB in conjunction with e.g. Liquid Rubber and other additives and waxes is proposed.
  • FIG. 1 Process diagram of a system for direct granulation of
  • Carbon Black Figure 2 is a block diagram of the CB post-bake
  • FIG. 3 shows a block diagram of the process sequences according to the invention in comparison to FIG. 2
  • FIG. 4 Summary of the functional sequences for the production
  • FIG. 5 shows the comparison of the procedures after the
  • a carbon black 29 (CB) of any origin or any manufacturing process can be introduced, in any case, it does not depend on the introduction of recycled carbon black.
  • the introduced via the input branch material flow is fed to a mill 2, which is preferably designed as a mechanical mill. It is an impact mill, with superheated steam of z. B. a temperature of 306 ° C with a mass flow of 507 kg / h and a pressure of 37 bar works. Again, these are preferred examples, which do not limit the subject invention.
  • This superheated steam 4 is introduced via the inlet 3 in the mill 2.
  • a refined granular stream of carbon black 29 is present, with a mixture of fine carbon black with a mean grain size of usually 2 ⁇ to 10 ⁇ in conjunction with the mixture of superheated steam.
  • This material flow is set in a certain ratio to the introduced at the input branch 9 mass flow, wherein z. B. a ratio of 1: 2 and the like can be provided.
  • the mass flow mixed with steam is fed via the input 6 to a condenser 8.
  • a number of additives 30 are supplied via the input branch 9, wherein the additives z.
  • Example have a temperature of 20 ° C and in the ratio of 2: 1 are introduced to the mass flow at the entrance 6.
  • additives is understood to mean a multiplicity of possible additives, such as, for example, water, silica, waxes, soot, chemicals, liquids of all kinds or liquid rubber.
  • water ice can be supplied or a partial stream of the already obtained slurry, even in frozen form.
  • the substances mentioned are introduced into the condenser 8 and sprayed there, because in a preferred embodiment it is a spray dryer.
  • the jacket of the spray dryer is designed as a cooling jacket 12 and to supply the cooling jacket 12, a cooling section 10 is provided via which the water z. B. with a temperature of 20 ° C and a pressure of 5 bar is supplied from a pump 1 1, which performs forced a jacket cooling and the output water finally a temperature of z. B. about 40 to 80 ° C has. This results in a substantial cooling of the introduced into the capacitor 8 substances.
  • the cooling is realized above all by metering in the additives, because the additive particles absorb the heat and cause a spontaneous condensation of the introduced gas mass flow.
  • a conveyor screw 13 driven by a motor 14 is arranged, which, however, may also be designed as a different type of conveying device. It is a longitudinal conveyor, which may also be formed in other ways, and it is assumed that at the entrance of the screw conveyor 13 is a temperature of about 80-90 ° C at a pressure of about 1 bar.
  • These screw conveyor 13 can be provided with a water cooling 15, so that the mass flow at the output 1 6 of the screw conveyor 13 has a temperature of about 60 ° C.
  • additives are fed into the extruder 17 via the input branch 20, these additives 31 being made of the same materials may exist as described above with respect to the additives 30.
  • the extruder 17 is a compression and mixing of the mixture in conjunction with the additives and in conjunction with the temperature control 19, which may be designed as cooling or heating, there is an expulsion of the still in the mixture of water, which via the output branch 21st is sucked with a pump 22 and possibly also contains gas fractions, which are removed as exhaust gas 23.
  • the granulation 25 essentially consists of a fixed perforated plate on which a rotationally driven knife passes, and the mass flow passes through the various holes of the perforated plate and is cut off by the passing knife.
  • Such granulators are standard devices in the plastics industry.
  • the drying 26 may be formed as a fluidized bed drying, as a spiral cooler or the like. Also of this drying 26 is an exhaust gas flow, which is introduced into the output branch 21.
  • the now dried and granulated mass flow reaches the outlet branch 27 and it is now present as the finished granulate 28 made of the carbon black 29 and the admixed additives. It is assumed that this granulate has a residual moisture content of ⁇ 3% at a temperature of less than 60 ° C. Possibly. is a post-refinement in a silo required.
  • the pump 22 can also cause a negative pressure in the output branch 21, which can lead to a vacuuming in the extruder and in the drying, so as to dissipate unwanted gas fractions.
  • the output of the grinding stage 32 opens into a filtration 36, where air filtration takes place with a complex air filter and the exhaust air 39 must be removed from this filtration stage.
  • the filtered product is a Verperlungspro 41 supplied, which consists of the prior art of a spiked roller, as described for example in EP 0 814 133 B1, with their operation and maintenance is associated with great effort.
  • a disadvantage of the prior art block diagram of Figure 2 is that the water 40 supplied to the sparger 41 must later be removed as steam 44 in the outlet branch 45.
  • the end product of the downstream drying stage 42 is likewise a pelleted carbon black 43, which, however, has a different composition than comparatively the carbon black in the form of the granulate 28 according to FIG. 1 of the invention.
  • This prior art carbon black 43 is heavily dust-laden, highly sensitive and difficult to process further. This is where the invention starts, which dispenses with such a starting product in the manner of the pelleted CB 43 and instead selects other process steps.
  • the pelleted CB 43 according to the prior art according to Figure 2 has a significantly lower bulk density than the comparatively obtained by the process of Figure 1 carbon black mixture 28, and this results in significant advantages.
  • it is proposed as a deviation from the block diagram according to FIG. 2 in FIG. 3 according to the invention that the complicated filtration is now replaced by a condensation stage 33. Otherwise, the same reference numerals and the same explanations apply to the same parts.
  • the drying stage 42 connects, and the previously introduced steam can now be removed as steam 44. Accordingly, the existing water is already evaporated here.
  • the pelletized carbon black (43 ') obtained in the inventive process scheme according to FIG. 3 has different properties than the carbon black shown in FIG. 2 in the prior art, because in FIG. 3 it is additionally stated that additives 30 are added in the condensation stage become.
  • the condensation in the condensation stage 33 is substantially improved, but then obtained as a pelleted carbon black 43 'is a carbon black-silica mixture.
  • the mixture of carbon black and additives obtained according to the process scheme according to FIG. 3 is designated by the reference symbol 43 '.
  • Advantage of the method according to Figure 3 is that already the additive in the condensation stage 33 has been added and a subsequent admixing is no longer required.
  • the carbon black 43 'obtained according to FIG. 3 has a significantly higher bulk density and improved processing capability than respectively compared to pure carbon black or pure silica.
  • FIG. 4 shows that the sputtering 41 and the drying 42 according to FIG. 3 are now replaced by an extrusion stage 34, as also shown in FIG.
  • Figure 1 illustrates the block diagram of Figure 4 in more detail, while in an alternative, a process flow of Figure 3 is possible.
  • Figure 4 shows the replacement of the Verperlungscare 41 and the drying stage 42 by an extrusion stage 34, where it can be seen that in the grinding stage 32, the carbon black 29 and steam 38 are introduced, as shown in Figure 3.
  • a pure carbon black or a recycled carbon black 62 may occur at the output of the grinding stage 32.
  • a carbon black may be introduced into the milling stage 32 according to any manufacturing process.
  • Such manufacturing processes are z. As a Furnace process, recycling process, pyrolysis process and the like.
  • condensation stage 33 At the output of the grinding stage 32, the introduction into the condensation stage 33, which has already been shown and described in detail in Figure 1 takes place. There, the condenser 8 was shown as condensation stage 33, to which the various auxiliary units shown in Figure 1 are assigned.
  • An extrusion stage 34 is then connected to the outlet of the condensation stage 33, wherein it is important that additives 30 can be introduced both in the condensation stage 33 and other or similar additives 31 in the extrusion stage 34.
  • the resulting pre-compound 28 is a granulate, as it was shown at the output branch 27 in Figure 1.
  • FIG. 5 summarizes the different alternatives of the present invention compared to the prior art.
  • FIG. 6a accordingly shows a standard process for the production of rubber according to the prior art, while the circumscribing circle relating to FIG. 6b represents a conventional process sequence according to the introduction to the description of DE 10 2012 105 796 B1.
  • FIG. 6c now shows the relationship of the present invention with the other process sequences.
  • FIG. 6a shows that soot production 46 of any type, such as, for example, can be produced.
  • B. can be done by a Furnace process, followed by the soot production 46 is a direct transfer 47 to a subsequent Verperlungswork 41.
  • the input branch 49 includes a first commercial stage because the production of pearlite and rubber production are separated in a second stage, production stage 55.
  • the known process sequence according to FIG. 6b shows a pyrolytic production stage 50 for the production of soot, in which waste rubber is recycled.
  • the process product produced in the intermediate stage 52 is a recycled soot B, which is present as a porous granulate B.
  • the porous granulate B is fed to the state of the art a Vermahlu and Verperlung 53.
  • the output branch 54 of the grinding and polishing 53 is in turn fed via the input branch 49 of the rubber production 55. It is characteristic of the process according to FIG. 6b that, in the intermediate stage 52, the intermediate material (recycled soot) obtained there can be fed via the input branch 51 to another production process for soot production 46. This is described in the mentioned patent DE 10 2012 105 796 B1.
  • FIG. 6c sets in which, in a preferred variant, for example, starting from a production stage 50 with a pyrolytic recycling of waste rubber, grinding and granulation of the substance is carried out directly without interposition of an intermediate stage 56.
  • the intermediate stage 56 corresponds to the input material 29 from FIG. 1.
  • the grinding and granulation is carried out with the production stages as described by reference numerals 32, 33 and 34 in the above description.
  • the porous granulate B from process 50 is stored in an intermediate stage 56 and possibly also transported and then fed to the process 32, wherein it does not matter in FIG. 6c that a direct transition from process 50 to process 32 takes place would.
  • the process 50 may be located at a different location than the process 32, which would allow the process 50, the process of FIG. 3 (32, 33, 41, 42) or FIG 4 (32, 33, 34) and the process 55 at three different Can be located, if this makes sense for an economic implementation of the procedure.
  • the process 55 may be identical to the process 106 or 103 in FIG. 7.
  • the starting product in the output branch 57 then appears as a pre-compound C having a defined composition, for example in the form of a free-flowing granulate having a particle size of 3 mm.
  • FIG. 7 shows the relationship between the measures according to the invention (right-hand illustration in FIG. 7) in conjunction with the process sequences according to the prior art.
  • the "invention 3" is shown on the right side, from which it follows that a pre-compound 105 is to be produced from various additives 31 of a rubber compound via an extruder 103 via the outlet branch 104, which then takes the form of granules 105 is added to the mixer 106 in batch mode in addition to other additives
  • the sum of the formulation ingredients added to the mixer 106 along with the pre-compound 105 along with the pre-compound 105 results in the rubber compound 108.
  • a main advantage is furthermore that via the intermediate step extruder 103, the additives 31 present in powdery or highly dusty form after extrusion as a pre-compound have a substantially higher density than the sum of the added additives 31. Since the mass of a mixture often exceeds the max. Filling volume of the mixer is limited by the introduction of the additives as pre-stabilized pre-compound the degree of filling of the mixer or increase the batch weight. Possibly. the total amount of an additive, e.g. As silica, which can be introduced into a batch, can be significantly increased, whereby an increase in performance of the mixing process and thus a higher efficiency and higher throughput of the entire mixer line can be achieved. This can lead to significant savings.
  • an additive e.g. As silica
  • This method is particularly suitable for incorporation of recycled carbon black 62 which has been prepared according to the measures of FIG. Reference is therefore made to reference numerals 48, 54 and 56 in FIG. 6 and to the description there.
  • the recycled carbon black (rCB) 62 may therefore optionally be fed to the extruder 103 or not. That is, it comes in the representation of Figure 7 only matter that the mixing process belonging to the prior art, an extruder is switched according to the invention, and the illustration in Figure 7 states that as additive to the extruder even a recycling Caron Black 62 can be supplied or additives, such.
  • the additives 31 which consist of carbon black and / or silica and / or waxes and / or liquids and / or liquid rubber and / or chemicals.
  • the invention 3 is to add an additional pre-compound via the output branch 104 in the prior art mixing process to make the mixing process more efficient, namely, to achieve a higher degree of filling for the mixer and an increase in performance to allow this mixer over the prior art.
  • the extruder 103 can now be placed in close proximity to the mixer 106 and the weighing and metering 107 and its pre-compounded added directly to the mixer. But it can also be further away and the pre-compound is supplied via a promotion of weighing and dosing 107 via the input branch 109 and passes in this way in the mixer 106th
  • the inventions 2 and 3 are combined and the extruder 17 of Figure 1 and the extruder 103 of Figure 7 are one and the same machine and the pre-compound 57 corresponds to the pre-compound 108 and is about the dosage and Weighing 107 fed to the mixing process.
  • the pre-compound 57 is one of the additives 31 of FIG. 7.
  • the pre-compound 104 would contain portions of the pre-compound 57 and the extrusion process 103 would be applied to the extrusion process 17 followed, wherein the extrusion process 17 is spatially separated in the vicinity of the pyrolysis process 50, whereas the extrusion process 103 is in the vicinity of the mixer 106 and there is a trade route C according to Figure 6c therebetween.
  • Figures 8 to 12 show different apparatuses used in the processes according to the invention.
  • a capacitor 8 is shown as an exemplary embodiment, which consists essentially of a container 63 having a cooling jacket 67 which is cooled by a coolant flow, not shown.
  • the cross-section of the container 63 is approximately conical and on its upper side an additive feed 64 is provided, which is formed by a task member 66.
  • the task member 66 may be a mixer, a feed screw or the like. It is important that in the container 63 is added to the product flow, which is introduced via the input 6, wherein on the outlet 77 emerging exhaust gas 78 is discharged.
  • the previously described screw conveyor 13 or another discharge member is arranged, and the mass flow prepared in the condenser 8 then leaves in the indicated arrow direction the output 1 6 of the screw conveyor 13th
  • a cyclone 88 can also be used in the process diagram according to FIG. 1, which is shown only in dashed lines as an optional feature.
  • the cyclone 88 according to FIG. 9 would then be arranged in the outlet branch 5 at the outlet of the mill 2 in front of the inlet branch 6 of the condenser 8 and in FIG. 9 consists of a container 89 into the interior of which the product stream is fed via the inlet 6. It passes through a quench 91 in which the additives 30 are also supplied via the inlet 7 in order to achieve a mixing with the mass flow at the inlet 5 there.
  • This premixed mass flow passes into the container 89, is circulated there according to the known mode of operation of a gas cyclone and set in rotation so that a partial flow with low particle loading via the gas outlet 92 as gas 93 separates.
  • the compressed partial flow forms a starting material 95 at the outlet of the cyclone container 68.
  • the use of a cyclone 88 shown in FIG. 9 in the process diagram according to FIG. 1 has the advantage that the mass flow at the discharge 94 has a higher charge than the starting material 95 comparatively according to the process scheme of Figure 1, in which the output of the mill 5 is guided directly into the condenser 8.
  • the concentration of soot in the granules 28 at the end of the procedure is significantly increased.
  • the gas 93 can not be described here in more detail by way of a separator for separating off the particles, and the gas consisting for the most part of water vapor can be supplied to the inlet 4 of the mill 2 after compression in order to further improve the overall energy balance of the process.
  • the arrangement of a quench 91, in which the additives 30 are supplied has the advantage that at the outlet 95 steam, droplets and gas are present in mixture form, whereby a particularly intensive mixing of the product is given.
  • FIG. 10 shows, as a further exemplary embodiment, a capacitor 71 which represents an alternative to the capacitor 8 in FIG.
  • the condenser shown in FIG. 10 essentially consists of a container 72, which has a cooling jacket 67 and into which a feed pipe 73 centrally opens, via which the mass flow 6 is introduced from the inlet 6 in the form of the starting material 95 and in turn overcomes the quencher 91 ,
  • the inlet pipe 73 can also be introduced at any other point in any way in the container so that the design of the container is taken into account and the circulation of the suspension is disturbed as little as possible. It is only important that the outlet of the inlet tube 73 is completely covered by liquid.
  • the mass flow thus passes after passing through the quenches 91 in the interior of the container 72 and there is evenly distributed as a suspension 74, wherein the suspension is present as a liquid medium in which the soot particles and additives and gas fractions are dispersed, and by the introduction of the feed tube 73 and the intensive contact with the suspension 74, the mass flow is cooled and flows through the liquid column of the suspension 74 and the gas component in the form of water vapor condenses completely to water.
  • Additives 30 can additionally be introduced into the suspension 74 via the inlet 76.
  • the suspension 74 is stirred by an agitator 75, which is driven by a motor and at the outlet 79 is then a slurry slurry (slurry), which is provided as a suspension 74 for further processing, as shown in the process scheme of Figure 1.
  • additives 30 leads to a further cooling of the suspension 74 and results in an improved degree of mixing into the suspension.
  • FIG. 11 shows an embodiment modified from FIG. 10, in which the capacitor 71 is shown in the left-hand illustration according to FIG. 11 and the same reference numerals and the same measures apply to the same parts.
  • the condenser 71 shown in FIG. 10 has at its outlet 79 a throttle 81 which opens into an inlet 82 which opens into a concentrator 80.
  • this concentrator 80 a further concentration of the suspension is achieved by sedimentation, evaporation of the water, or other suitable methods.
  • the previously prepared suspension 74 is converted into a compacted suspension 74 'by either cooling or heating alternatively via the temperature control jacket 67', thus evaporating water the suspension 74 ', wherein this water is discharged via the discharge line 85 as water vapor and a filter 86 is supplied to which a pump 87 is arranged, which discharges the steam 98 into the environment.
  • the filtered-out in the filter 86 substances are recycled via the discharge member 96 again as a particle mixture 97 the further process.
  • the discharged particle mixture 97 may, for. B. in the form of an additive in Figure 10 at reference numeral 30 are fed again.
  • the steam 98 at the outlet end of the pump 87 can be used as process steam at the steam jet mill 2 according to FIG. This results in a significant improvement of the energy balance.
  • suspension 74 ' is kept in motion with an agitator 75 and discharged via the outlet 84 and the throttle 69 as suspension 74' and fed to the downstream process extruder 17 via access 1 6 according to FIG.
  • the suspension 74 'according to FIG. 3 can be fed to a shot 41 and to a drying 42 in order to produce a pelleted carbon black 43'.
  • the pressure level P1 on the condenser 71 is different than the pressure level P2 on the concentrator 80.
  • FIG. 100 An aggregate state curve, wherein a dividing line 99 is drawn, above which the mass flow is vaporous and below which the mass flow is liquid. Furthermore, a pressure curve 101 and a temperature curve 102 are shown.
  • the said curves are shown in different process steps of the running process.
  • the process steps are indicated by reference numerals 2, 91, 8, 63, 67, 80 and 74, respectively.
  • a quench 91 consists in principle of a piece of pipe which is flanged into the feed line and has the annularly arranged nozzle elements, via which a liquid or a suspension can optionally be injected with auxiliary medium pressure air in the interior. It can be used to cool mass flows of high temperature to low temperatures.
  • the temperature and pressure curve then opens into the starting product, which is present as a sludge-like water mass flow in the form of the suspension 74 'or 74.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

L'invention concerne un procédé pour la préparation de noir de carbone (NC), en particulier de noir de carbone recyclé, et un procédé de fabrication destiné à la fabrication d'un prémélange, consistant en les étapes suivantes : a.) fourniture d'un granulé sec de noir de carbone (NC) obtenu par un procédé pyrolytique b.) broyage du granulé de noir de carbone dans un processus de broyage à sec, une obtention directe de perles de NC étant réalisée à partir d'un broyeur (2), tout en évitant l'étage de filtration par une condensation du gaz porteur. c) extrusion et façonnage en aval, avec obtention d'un matériau commercialisable stable, ne dégageant pas de poussière, présentant une masse volumique et une stabilité plus élevées que celles du noir de carbone, qui est obtenu sous forme d'un granulé, d'un flexible, d'une chenille ou d'une nappe (bande plate continue). d) introduction de ce matériau sous forme de prémélange dans un mélangeur de caoutchouc, un gain important de rendement pouvant être atteint grâce à la charge plus élevée possible du mélange et l'augmentation du débit.
PCT/EP2017/083239 2016-12-28 2017-12-18 Procédé de préparation de noir de carbone et procédé de fabrication d'un prémélange pour une installation de mélange de caoutchouc WO2018122017A1 (fr)

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DE102016015591.4A DE102016015591A1 (de) 2016-12-28 2016-12-28 Verfahren zur Aufbereitung von Carbon Black und Herstellungsverfahren eines Pre-Compounds für eine Gummi-Mischerei

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CN108970268A (zh) * 2018-09-14 2018-12-11 中策橡胶集团有限公司 一种密炼机废气收集和处理系统
CN109111766A (zh) * 2018-09-08 2019-01-01 山东联科新材料有限公司 一种橡胶制品专用炭黑的生产方法
EP4137533A1 (fr) 2021-08-20 2023-02-22 Continental Reifen Deutschland GmbH Procédé de fabrication en continu de matières de départ pour la fabrication de pneus

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DE102020209826A1 (de) 2020-08-04 2022-02-10 Continental Reifen Deutschland Gmbh Vorrichtung zur Herstellung eines Kautschukmischung und deren Verwendung
EP4043536A1 (fr) * 2021-02-12 2022-08-17 Bernhard Grimm Dispositif et procédé de traitement humide du noir de carbone

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EP0924268B1 (fr) 1997-12-18 2003-07-09 Degussa AG Noir de carbone sous forme de perles et procédé pour sa préparation
WO2015089248A1 (fr) * 2013-12-13 2015-06-18 Ch2E California Llc Dépolymérisation du caoutchouc et procédés associés
DE102012105796B4 (de) 2012-06-29 2016-01-21 Pyrolyx Ag Verfahren und Vorrichtung zur Herstellung von Hybrid - Carbon Black - Teilchen

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US3740861A (en) * 1970-06-17 1973-06-26 Cities Service Co Method for drying carbon black pellets
DE2641187A1 (de) * 1975-10-01 1977-04-14 Goodyear Tire & Rubber Verfahren zur herstellung von russ
US4296800A (en) * 1980-04-18 1981-10-27 Phillips Petroleum Company Waste heat recovery
EP0814133B1 (fr) 1996-06-11 2000-02-02 Degussa-Hüls Aktiengesellschaft Procédé pour la granulation sèche en continu de noir de carbone
EP0924268B1 (fr) 1997-12-18 2003-07-09 Degussa AG Noir de carbone sous forme de perles et procédé pour sa préparation
DE102012105796B4 (de) 2012-06-29 2016-01-21 Pyrolyx Ag Verfahren und Vorrichtung zur Herstellung von Hybrid - Carbon Black - Teilchen
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CN109111766A (zh) * 2018-09-08 2019-01-01 山东联科新材料有限公司 一种橡胶制品专用炭黑的生产方法
CN109111766B (zh) * 2018-09-08 2020-11-17 山东联科新材料有限公司 一种橡胶制品专用炭黑的生产方法
CN108970268A (zh) * 2018-09-14 2018-12-11 中策橡胶集团有限公司 一种密炼机废气收集和处理系统
CN108970268B (zh) * 2018-09-14 2023-06-23 中策橡胶集团股份有限公司 一种密炼机废气收集和处理系统
EP4137533A1 (fr) 2021-08-20 2023-02-22 Continental Reifen Deutschland GmbH Procédé de fabrication en continu de matières de départ pour la fabrication de pneus
DE102021209200A1 (de) 2021-08-20 2023-02-23 Continental Reifen Deutschland Gmbh Verfahren zur kontinuierlichen Herstellung von Ausgangsmaterialien für die Reifenherstellung

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