WO2018122017A1 - Method of processing carbon black and production process for a pre-compound for a rubber mixing plant - Google Patents

Abstract

A method of processing carbon black (CB), especially recycled carbon black, and a production process for the production of a pre-compound consisting of the following steps: a.) providing a dry pelletized material composed of carbon black (CB) from a pyrolytic method, b.) grinding the pelletized material composed of carbon black in a dry grinding process, wherein direct beading of CB from a mill (2) takes place with avoidance of the filter stage as a result of condensation of the carrier gas, c) downstream extrusion and shaping, wherein a saleable stable, non-dusting material with relatively high density and stability is obtained in the form of carbon black, obtained in the form of pellets, tube, bead or sheet (flat, continuous strip), d) feeding this material as a pre-compound into a rubber mixer, wherein the higher possible loading of the mixer and increase in the throughput can achieve a considerable efficiency gain.

Description

 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.

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.

In the recycling of waste rubber by a pyrolytic process is usually a dry granules with a very high proportion of CB at. Usually, this granulate is ground in a mill to prepare it into a workable recycling raw material. The fine powder obtained in this grinding process must then be processed in a further operation to pearl carbon black in order to be able to supply it to a commercial chain. This shot usually follows the same procedure as used in other commercial production processes for technical carbon blacks.

The carbonation of 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.

When recycling CB (rCB) is processed, the starting material today is first comminuted by a mill. Here air jet mills are usually used. The powder thus produced is then separated via a filter from the gas stream. The filter stages are expensive and the resulting filter dust is difficult to handle. The resulting filter dust is then usually fed to the batch. For this purpose, the Trockenverperlung or Wetverperlung is generally known. Due to the higher achievable pearl hardness, the wet batching process is common. In wet sputtering, the dry matter is mixed with water (about 40 to 60% by weight, based on the total mass) and fed to the sputtering. The setting of a suitable pearl hardness is of crucial importance for further use here. Subsequently, the supplied moisture must be removed in an energy-intensive process again. Frequently, 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.

The prior art cf. et al Patent "Pearl Soil and Process for Producing EP 0 924 268 B1" A process for the continuous dry granulation of powdered carbon black is described by the subject matter of EP 0 814 133 B1 This publication describes the known process step of dry granulation of carbon black the local description is made in addition to the explanation of the present invention description.

This document also describes the so-called wet granulation, and the two granulation processes are compared. It can be seen from the document that a complex batching is necessary, which is associated with a high level of machine outlay and uses a considerable amount of additives and auxiliaries which remain in the carbon black. However, even with well-soaked soot, there is still a product that is prone to dusting and must be handled with the utmost care to minimize contamination of the black dust environment. Likewise, the pearl carbon black must be handled with care to minimize breakage of grain and the production of further fines, which is disadvantageous for further use.

Another disadvantage of wet sputtering is the necessity of using water, and the water has to be removed again at a later stage of the process.

The subject of 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).

Incidentally, this document also discloses the fact that waxes and other additives are added, and reference is made to Figure 2 of the present invention, where this known method is shown graphically.

Disadvantage of the known method is therefore the need for the arrangement of a Verperlungsstufe and the supply of water and its subsequent energy-consuming removal from the process. As a starting point of the spell, a Pearl Russ is created. The associated disadvantages have been described above with reference to EP 0 814 133 B1. The introduction of such a pearl soot in the later, industrial mixing process is greatly hampered by an increased fines. On the one hand, a higher proportion of fines makes for a disadvantageous formation of dust and difficult handling of the CB, in particular during the conveyance and weighing of the CB, upstream of a mixing process. On the other hand, the bulk density is reduced, which can adversely affect the possible capacity of subsequent mixing processes. 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 solution of the problem is achieved by the technical teaching of at least one of the independent claims.

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.

Another advantage of the invention is that the pre-compound (PCO) prepared according to this process can be packaged and delivered much better, easier, cheaper and dust-free than merchandise. Due to its usually greater stability and bulk density, it may in return to percolated CB transported, stored and metered with less logistical effort.

In addition, neither grain breakage, fines formation or strong dust development with a corresponding disadvantageous effect on the logistics process are usually to be expected. Despite the significantly larger and more stable grain compared to the pearl butter, no negative effects on the dispersibility of the pre-compound in the rubber compound during the mixing process are to be expected.

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.

In addition, the degree of dispersion of the additives in the mixer can be improved, which was previously not possible in the prior art.

A disadvantage here could be considered that the pre-compound in addition to the soot contains a significant proportion of other substances that are added to the mixing process in this composition and thus allegedly hindered the flexibility in the recipe design of individual rubber compounds. 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. On the other hand, it is still possible to supplement other additives during the mixing process, so that a pre-compound usually brings only a subset of a recipe ingredient in the mixture and the necessary amount to achieve the desired recipe is complemented conventionally, so that the full flexibility of Recipe design is preserved. However, the required amount to be supplied per mixture becomes various recipe ingredients reduced, whereby these dosing are relieved or possibly bottlenecks can be eliminated.

Although with the subject of DE 10 2012 105 796 B4 a method and an apparatus for the production of hybrid carbon black particles has become known, which is characterized in that a product granules based on carbon in several heating zones with different temperatures in one Pyrolysis is pyrolyzed to a pyrolysis product, wherein the product granules in each heating zone lingers for 4 hours. Two different production streams are formed.

After the second carbon black base particles have been ground, 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.

Disadvantage of the known method, however, is that the admixture of the second carbon black base particles in the flow of the first carbon black base particles is associated with high difficulties and throttles the process of supplying the first carbon black base particles and makes it difficult.

After admixture of the second carbon black base particles in the first particle stream, the other procedure according to the state of the art must be carried out, namely the filtration, beating and drying, as shown as prior art in the flow chart of Figure 2 of the present invention.

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. Incidentally, 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. According to 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.

Accordingly, the present invention provides the following partial inventions, each of which should enjoy protection for each other individually but also in any combination:

1.) Condensation from the vapor phase without filter stage after dry grinding. 2.) The quenching with additives if necessary in addition to water to support a spontaneous condensation.

3.) The process of producing a pre-compound is not today established in the rubber market on a larger scale.

4.) Incorporation of CB recycled goods through a logistic process with the rubber industry is more economical than previous approaches. The process presented here could be a commercially successful way of making a recycling cycle for recycled CB marketable. The production of precompound in the rubber industry is seen as the logical next step for the production of rubber. This technology is not limited to use on recycled goods.

The invention comprises several steps whose individual steps should enjoy protection both alone and in any combination with one another.

In a first step, the previous investment-intensive filter stage can be significantly reduced.

In the second step, this energy-intensive treatment process can be energetically optimized significantly.

In a third step, the condensation of water vapor is supported by quenching with additives.

In a fourth step, a new form is created as a commercial product.

Through a process optimization, a pre-compound is to be produced, which can be handled much easier than pearl tufts and also shows many other advantages.

Finally, in a fifth step for the production of the merchandise, the usual today Verperlungsmaschine be replaced by an extruder that produces much larger and much easier to handle beads.

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. For this purpose, 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). After grinding, 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 Verperlungsstufe. The heat of condensation is used to generate new steam.

Part 2 - Energetic total balance

So far, in the rubber recycling process, the production of recycled carbon black and the tempered CB treatment process are considered as two separate process steps. 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. Also, 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.

1 . Variant of Part 2:

The pyrolysis product is not cooled after pyrolysis, but fed directly hot steam jet mill. To accelerate the feed to the steam jet mill, an injector is used. 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. 2nd variant of Part 2:

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. Part 3 - Quenching of the wet steam stream with additives and Impfqut for spontaneous and complete condensation of the vapor phase - Addition of additives for spontaneous cooling of the mass flow 3.1 The recycling CB (rCB) is in the steam jet mill to particles between 2 μηι and 10 μηι milled. The particle vapor stream from the steam jet mill is fed in a preferred embodiment, first in a stage for precooling. In this case, 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. By suitable choice and control of the pressure level over the entire procedure and the reduction of the pressure at a suitable place in the process the place of the condensation is skilfully influenced.

3.2 In a preferred variant, 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.

3.3 In one variant, 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. As a result, the amount of additives required for complete condensation of the water vapor is reduced, thereby increasing the proportion of CB in the end product.

In this case, it may be advantageous in a further embodiment variant to first conduct the gas stream via a gas cyclone. Thereafter, the gas stream with fine particles of a filter stage is fed while the gas stream with the coarse particles is fed directly to the condensation.

3.4 In a variant of this, 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. In this case, the fineness of the Aufmahlung or the product quality can be influenced.

Which embodiment is ultimately preferred, investment and operating costs must be decided on the one side, product quality and composition on another page, as well as plant complexity and reliability and efficiency on the third corner of the triangle in the conflict of objectives triangle. 3.5 In order to accelerate the cooling or the condensation of the vapor phase after the milling, additives of low temperature are added to the precooled wet steam particle stream, which are used anyway in the later rubber mixture. The introduction of the cooler additives results in a lower mixing temperature. As a result, a spontaneous cooling of the wet steam and a condensation of the steam can be achieved.

In addition, the additives can positively influence the formation of the beads (condensation nuclei) or the strength of the beads.

It is considered advantageous that the incorporation of the additives via spray heads has a uniform mixing with the wet steam particle flow result and thus already here a homogeneous mixing of various additives of a rubber compound can be achieved without supplying further mixing energy. This proves to be advantageous in achieving a homogeneous distribution of the additives in the later rubber compound.

Part 4 - Production of a Pre-Compound (POC) The additives are added to a far greater extent than would be required for the normal carbonization process of the carbon black. Here, for example, 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. In addition, 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.

This or other metered substances cause the following effects or have the following properties:

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. For this purpose, it may be useful to subdue the substances to be metered, for example by grinding in the case of solids or by spraying liquids. it is desirable to increase the level of carbon black in the final product. Thus, 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. In one variant, 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.

Throughout the entire process, 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.

In order to enable a clean temperature-pressure-guidance in the process, 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 premixing and thermal treatment of these substances by the process shown in this mixture does not lead to a negative effect on the development of properties that this additive in the recipe according to the original method used to unfold.

Ideally, 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. Ideally, 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.

Part 5 - Replacement of the beading machine by an extruder

The extruder instead of the granulation optimizes the mixing of the different feedstocks. The addition of further additives is conceivable and intended. By means of a granulation stage, beads can be produced which have excellent transport logistical properties. The bulk density of the beads is higher than that of the sum of their additives and thus the efficiency of the rubber mixer can be increased. Under an extruder, the invention means a machine with one or more, rotating in a channel, screw-like spindles with patch mixing elements of various designs. Such 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 result is the following advantages:

The filter stage is completely eliminated => high investment and operating cost advantage, reduced space requirements of the plant.

The use of steam as a carrier medium for grinding reduces energy costs. The cooling process downstream of the process returns part of its energy to the evaporation process. In contrast, the energy of a prior art air jet mill is lost through the process. Part of the cooling is taken over without the use of energy by the introduction of other substances. Part of the heat energy for the production of the required steam is introduced from the still hot and not cooled recycling CB.

The handling of pre-compound is easier than pearl pearl or

Silica. · 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. · Due to the higher density of the new pre-compound compared to the sum of the volume of its components as individual feeds, the mixer (e.g., an internal mixer for rubber in batch mode) 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.

Since some of the aggregates are introduced into the process via the pre-compound, the additional dosage of the remaining amount of additive required to set the recipe quantity requires less time and effort. This has a positive effect on the handling effort and in a favorable case on the cycle time and the dosing accuracy. If necessary, bottle-neck in the area of dosage and weighing up-stream can be eliminated. The invention will now be described by way of a brief summary of its features as follows: 1 . Granules from a thermal recycling plant for rubber are used in the temperature range between 10 and 500 ° C.

2. superheated steam is used instead of air or combustion gases as a carrier medium for grinding.

3. 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. In addition, the proportion of different configurations of gas cyclone and / or filters can be favorably influenced.

In a preferred embodiment, the recycled soot is milled to a mean particle size of between 1 and 6 μm 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.

4. 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.

5. The added additives are anyway components of the formulations of the further processing of the product. 6. 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.

8. In the extruder before granulation, 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.

9. 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. When using recycled CB thus results in a fluctuation in the composition of the branch 1 6 the extruder 17 supplied product (see Figure 1). In the extruder before granulation, 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 different aspects of the invention are shown again as follows:

1 . Direktverperlunq

Process for the direct suspension of CB from a jet mill while avoiding the filter stage by condensation of the carrier gas characterized by one or more of the following characteristics in any combination with each other: a gas-solid mixture in which the solid fraction is dispersed as fine particles in the gas stream. Usually, gas and solid by z. As filters or cyclones separated from each other. This condition is usually obtained z. B. after a jet mill. In the case of a simple jet mill, an air-solid particle mixture is present, in the case of a steam jet mill, a water vapor solid particle mixture is present.

 - Instead of an alternative separation technology (filter, cyclone, scrubber), the gas stream is condensed according to the invention. The condensed gas is then evaporated again from the solid.

 - To support the rapid condensation, 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. premix

Preparation of premixes of silica and CB in combination with liquids and waxes for easier handling in the mixing process and increase the mixing throughput and the mixer efficiency.

3. 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.

The advantage of this invention idea is that the introduction of substances makes it possible to cool a mixture more quickly. This makes it clear that with relatively little effort a favorable production with low energy input is possible. The subject of the present invention results not only from the subject matter of the individual claims, but also from the combination of the individual claims with each other. All information and features disclosed in the documents, including the abstract, in particular the spatial design illustrated in the drawings, are claimed to be essential to the invention insofar as they are novel individually or in combination with respect to the prior art. In the following the invention will be explained in more detail with reference to drawings showing only one embodiment. Here are from the drawings and their description further features essential to the invention and advantages of the invention. Show it:

Figure 1 Process diagram of a system for direct granulation of

 Carbon Black Figure 2 is a block diagram of the CB post-bake

 State of the art

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

 a pre-compound for the rubber industry according to the invention

Figure 5 shows the comparison of the procedures after the

Prior art (left column) compared to the procedures according to a first embodiment of Invention (middle column) and a second embodiment of the invention (right column) schematic process representation of a standard process for the rubber production according to the prior art, a process scheme for rubber production according to

the aforementioned DE 10 2012 105 786 B1 a process sequence according to the invention in comparison to the above-mentioned other process sequences in Fig. 6a and 6b, the representation of a process flow with the method steps of the prior art (left part) and the representation of the method steps ( Right part) a preferred embodiment of a condenser device in the manner of a cyclone as a variant for carrying out the process according to the invention schematically the representation of a capacitor which is advantageously used in the inventive method is compared to Figure 10 modified embodiment with a two-stage capacitor and a Downstream Aufkonzentrierer a state diagram, pressure and temperature diagram of the process product over various stages of manufacture FIG. 1 shows a process scheme according to the invention in which the CB recycle granules 29 (rCB) are introduced at the input branch 1, an exemplary statement being that this carbon black 29 has a temperature of 200 ° C. at a mass flow of 100 kg / h and

has a bulk density of 640g / l.

It is a porous granules, which is comparable to a granulate from a spray drying.

Instead of the introduction of recycled carbon black (rCB), 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.

As a result of the meeting of the highly stressed steam particles on the granular stream of the carbon black 29, the particles of the carbon black 29 collide with one another and these are thereby broken up and crushed.

At the output branch 5 of the mill thus a refined granular stream of carbon black 29 is present, with a mixture of fine carbon black with a mean grain size of usually 2μηι to 10μηι 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.

In dashed lines it is shown that, as an additional variant of the idea of the invention in the branch 5, 6, the starting material of a cyclone 88 can be introduced.

The mass flow mixed with steam is fed via the input 6 to a condenser 8.

At the other input 7, 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.

The term "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.

Likewise, 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.

This results in a condensation of the introduced mass flow and at the outlet of the condenser, a suspension (slurry), which consists of a liquid phase with dispersed carbon black particles and the additives mixed with it.

At the output of the condenser 8, 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.

This mass flow is now introduced into an extruder 17, which is driven by a motor 18.

In addition, further 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.

In 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.

At the exit of the extruder 17 there is then a substance mixture which has a temperature of about 100 ° C., and at the outlet 24 this substance mixture is approximately pasty and is fed to a granulation 25. 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.

As a result, granules are formed from the pasty mass, which are then fed to a downstream drying 26. 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.

At the exit of the drying 26, 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.

This also supports drying.

The advantage of the method according to the invention according to FIG. 1 is compared with the prior art according to FIG.

According to the state of the art according to FIG. 2, it is known to first supply the carbon black 29 to a grinding stage 32, whereby this grinding stage additionally has to be supplied with compressed air 37.

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.

Thereafter, the filtered product is a Verperlungsstufe 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.

With this device, as described in Figure 1 of this document, a much larger machine cost than comparatively the method according to the invention according to Figure 4, connected. 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. In a development of the present invention, 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.

Advantage in the invention of Figure 3 is that in the grinding stage 32 instead of air 37 steam 38 is supplied, which is associated with the advantage that the grinding with steam has a higher efficiency and that the steam can then be condensed, namely in the condensation stage 33 according to the invention, and not - as in the prior art Technique according to Figure 2 - first water is supplied, which later must be removed as steam with high energy expenditure.

According to the flowchart according to the invention according to FIG. 3, it is therefore provided that, following the condensation stage 33, a sputtering 41 takes place, but without the supply of water 40, as was necessary in the prior art according to FIG.

The necessary in the Verperlungsstufe 41 water is replaced by the steam 38, which is obtained in any case in the condensation 33 as water and therefore can be used cheaply in the Verperlungsstufe 41.

This results in a much better energy balance in the flowchart of FIG. 3 in comparison to the flowchart of the prior art according to FIG. 2.

At the output of the Verperlungsstufe 41, 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.

For example, if silica is added as an additive, 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. For this reason, 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.

Another advantage is that 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.

In contrast to the process diagram according to FIG. 3, 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.

Accordingly, it follows that Figure 1 illustrates the block diagram of Figure 4 in more detail, while in an alternative, a process flow of Figure 3 is possible.

Accordingly, Figure 4 shows the replacement of the Verperlungsstufe 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.

Therefore, a pure carbon black or a recycled carbon black 62 may occur at the output of the grinding stage 32. Thus, both mixtures are possible. Accordingly, 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.

All carbon black particles which can be produced by the abovementioned processes can thus be supplied to the grinding stage 32.

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 number and composition of the additives has already been mentioned previously, and any selection of additives can be introduced both in the condensation stage 33 and 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.

In the left column of Figure 5, the prior art is shown, as has been described in detail in Figure 2. This description also applies to FIG. 5 (left column). In the middle column of Figure 5, the block diagram of Figure 3 is shown in principle, and in the right column of Figure 5, the block diagram of Figure 4 is shown. The same reference numbers apply to the same parts.

The comparison of the columns in Figure 5 results in the simplification of the method according to the invention, wherein either according to the "invention 1" the filtration 36 is replaced by a condensation 33 or - according to the "invention 2" and the Verperlungsstufe 41 through the drying stage 42 an extrusion stage 34 are replaced.

Both embodiments "Invention 1" and "Invention 2" should be taken for self-protection alone, but they should enjoy protection in any combination with each other.

This process comparison is again shown in FIG. 6, the relationship of the process sequences being represented by different boundary circles and the process sequence being supplemented by the downstream production of a rubber mixture 55. This production process of a rubber mixture is usually carried out in an internal mixer or extruder, into which, in addition to a multiplicity of further additives 58, 59, 60, 61 and bubbled carbon black 43, is added at the inlet 49. Usually, the production of carbon black (43) and the rubber production (55) takes place in different establishments whereby a trade route is required. The usual commercial form according to the prior art is pearlite (A). This pearlite has the problematic properties already shown in FIG. According to the invention, the amount of CB supplied is supplemented via the trade route A or reduced by precompound according to trade route C, whereby decisive advantages can be achieved. 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.

Accordingly, 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 Verperlungsstufe 41.

At the output branch 48 of the Verperlungssufe 41 then there is a bead A, which is usually supplied via a long trade route of rubber production 55 via the input branch 49.

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.

This is where the invention according to 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. In this embodiment, 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.

In an alternative embodiment, 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.

Rather, there may be a trade route between them and 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.

However, it can also be produced in the form of a hide or a hose or in another extruded form and can be supplied in this production form as a pre-compound C of the rubber production 55, but it does not depend on the shape, but that it easy to handle, store, transport and bring into the mixing process 55.

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. In FIG. 7, 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.

This has the decisive advantage that raw materials are transferred to the mixer in a predispersed state, whereby the mixing work in the mixer 106 is reduced and the homogeneous distribution of the additives 31 in the rubber mixture is favored. Material losses via aspiration and thus an uncontrolled falsification of the mixture is largely avoided.

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.

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. As the additives 31, which consist of carbon black and / or silica and / or waxes and / or liquids and / or liquid rubber and / or chemicals. Thus, it will be appreciated that 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.

Thus, a higher degree of dispersion of the additives in the rubber mixture of Figure 7 (left column) is achieved because the additives 31 are admixed and predispersed in an extruder 103 according to the invention.

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

In a particularly advantageous embodiment, 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. In a variant that may be advantageous in certain processes, the pre-compound 57 is one of the additives 31 of FIG. 7. As a result, 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.

In Figure 8, 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.

At the outlet 68 of the container 63, 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

As an additional process stage, 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.

Thus, the concentration of soot in the granules 28 at the end of the procedure is significantly increased. Moreover, 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.

This achieves a higher loading of soot in the mass flow and at the inlet 6 of the condenser.

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.

The working and energy capacity of the subsequent cooling stage (condenser) is thus reduced. 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 ,

In a variant, it is also possible to feed the output 5 of the mill 2 directly to the capacitor 71 according to FIG.

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.

It is crucial that the pressure and the temperature in the container 72 are controlled so that on the one hand a suitable supply via the input 6 is ensured and the other via the input 6 in the Container introduced water vapor almost completely condensed out to water.

The remaining residual gases are removed through the outlet 77 as exhaust 78. 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.

The addition of 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.

Thus, it can be seen from FIG. 11 that 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.

In this concentrator (thickener) 80, a further concentration of the suspension is achieved by sedimentation, evaporation of the water, or other suitable methods. Thus, 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.

Depending on the method, the 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.

In a variant, 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'.

Importantly, the pressure level P1 on the condenser 71 is different than the pressure level P2 on the concentrator 80.

It is P1> 1, 1 x P2.

These relationships are shown as a state diagram in FIG. It is represented by the reference numeral 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.

With reference to the state of aggregate curve 100, it can therefore be seen in FIG. 12 that before the steam jet mill, the mass flow is vaporous and remains vaporous even in the steam jet mill. He therefore leaves the steam jet mill 2 as a vapor and it is then converted by a quench 91, as shown for example in Figure 10 and 1 1, from the state of the vapor in the limit state for condensation, while the pressure of 37 bar behind the quencher 91 drops to a pressure which is shown at the curve 101 and at the same time the temperature of z. B. 500 ° C to a much lower temperature of z. B. drops below 120 ° C.

It should also be pointed out that a quench 91 could also be used in the process diagram according to FIG.

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.

It can also be seen from the illustration in FIG. 12 that the condensation point is already reached in the quench 91 and that a mixture of gas, droplets and suspension is now present in the condenser or a suspension and a further reduction in pressure and temperature takes place in the condenser 71 , Next, it can be seen from Figure 12 that in the evaporator or thickener 88, a partial conversion of the water to a vapor state takes place, but still the pressure and temperature are lowered. It splits off a partial mass flow of evaporated water, a part of the water remains liquid in the suspension 74 '.

By the approach of the throttle 81, the pressure level P1 is lowered relative to the pressure level P2 in the concentrator 80. This leads to an evaporation with a expulsion of steam - as shown in Figure 1 1 - and a concentration of the suspension, which is thus converted into the concentrated suspension 74 '.

This takes place on the vertical line in FIG. 12 at reference numeral 80.

After the further reduction of the pressure and the temperature, 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.

For realizing the procedure, it is also preferred in FIG. 11, in each case, to use a throttle 69 in the illustrated branches. 

Zeichnunqsleqende

1 input branch

 2 mill

 3 entrance

 4 steam

 5 output branch

 6 entrance (fabric)

 7 entrance

 8 capacitor

 9 input branch

 10 cooling section

 1 1 pump

 12 cooling jacket

 13 screw conveyor

 14 engine

 15 water cooling

 16 output (from 3)

 17 extruders

 18 engine

 19 temperature control

 20 input branch

 21 output branch

 22 pump

 23 exhaust

 24 output

 25 granulation

 26 drying

 27 output branch

 28 granules

29 carbon black additives

additives

milling stage

condensation stage

extrusion stage

additives

filtration

air

steam

exhaust

water

Verperlungsstufe

drying stage

Pelleted CB

steam

outlet leg

carbon black production

remote

output branch

input branch

production stage

input branch

intermediate stage

Milling & beating

input branch

 Production stage (rubber production) Intermediate stage

output branch

silica

 rubber

waxes

Liquids & additives Recycled carbon black

container

additive feed

arrow

feeding devices

Cooling jacket 67 '(tempering jacket) outlet

Choke capacitor

container

feed pipe

Suspension 74, 74 '

agitator

inlet

outlet

exhaust

outlet

Aufkonzentrierer

throttle

Intake

container

procedure

discharge

 filter

 pump

cyclone

 container

 product input

 quench

 gas output

gas 94 discharge

 95 starting material

 96 discharging organ

 97 particle mixture

 98 steam

 99 dividing line

 100 aggregate state curve

 101 pressure curve

 102 temperature curve

 103 extruders

 104 output branch

 105 pre-compound

 106 Mixing process for rubber / internal mixer for rubber

 107 Weighing and dosing of rubber compound feedstocks

108 rubber compound

 109 pre-compound

Claims

claims

1 . Process for the preparation of carbon black (CB), in particular recycled carbon black, and a production process for the preparation of a pre-compound, comprising the following steps:

a. ) Provide a dry granular carbon black (CB) pellets from a pyrolytic process

b. ) Grinding the granules of carbon black in a dry grinding process

characterized in that a Direktverperlung of CB from a mill (2) takes place while avoiding the filter stage by condensation of the carrier gas.

2. Process for the preparation of carbon black (CB), in particular recycled carbon black and a production process for the production of a

Pre-compounds consisting of the following steps:

a. ) Provide a dry granular carbon black (CB) pellets from a pyrolytic process

b. ) Grinding the granules of carbon black in a dry grinding process

characterized in that

b1.) the grinding of the granules in process step b.) With superheated steam

b2.) And that in a subsequent process step, the vapor-particle mixture is passed through a cooling stage, in which the vapor condenses out.

3. Process for the preparation of carbon black (CB), in particular recycled carbon black and a production process for the preparation of a pre-compound comprising the following steps:

a.) Providing a dry granules of carbon black (CB) from a pyrolytic process b.) grinding the granules of carbon black in a dry grinding process

wherein a Direktverperlung of CB from a mill (2) takes place while avoiding the filter stage by condensation of the carrier gas.

c) downstream extrusion and shaping to produce a stable, non-dusting, high-density and stable-than-carbon stable commercial material which is in the form of granules, tubing, caterpillar or hide (flat, continuous band).

d) feeding this material as a pre-compound in a rubber mixer, which can be achieved by the higher possible loading of the mixer and increasing the throughput, a significant efficiency gain.

4. The method according to any one of claims 1 to 3, characterized in that

a.) The obtained from the pyrolysis dry granules in the hot state of a steam jet mill is added and

b.) the heat energy of the granules is used to generate steam.

5. The method according to any one of claims 1 to 4, characterized in that in step b1.) After cooling or condensation obtained pre-cooled wet steam particle stream additives are added to accelerate the cooling or the condensation of the vapor phase after grinding,

6. The method according to any one of claims 1 to 5, characterized in that the obtained at the output of step b2.) Material is a pre-compound, which can be processed after the expulsion of excess water to a stable granules.

7. The method according to any one of claims 1 to 6, characterized in that the steam used in step b1) as a carrier medium for the Milling is used by the heat obtained in the downstream cooling process.

8. The method according to any one of claims 1 to 7, characterized in that the gas / soot particle mixture is treated via a filterless process to steam just above the saturated steam region with a weight fraction of soot particles between 0.1 and 50 wt .-%.

9. The method according to any one of claims 1 to 8, characterized in that the multicomponent mixture obtained in step b2.) Is supplied with a high proportion of water optionally a batch in a beading machine and / or a further processing in an extruder.

10. The method according to claim 9, characterized in that in a further processing in an extruder further substances are added, wherein the mass is mixed intensively and the heat of vaporization of the outgassing water contributes to the cooling of the mix in the extruder.

1 1. Apparatus for processing carbon black (CB), in particular recycled carbon black (rCB), consisting of the following

Device components:

a. ) Device for producing a dry granulate of carbon black (CB), preferably from a pyrolytic process

b. ) Mill for grinding the granules of carbon black in a dry grinding process

characterized in that

the grinding of the granules in process step b) takes place with superheated steam in the mill (2).

12. The device according to claim 1 1, characterized in that the mill (2) is designed as an impact mill.

13. The apparatus of claim 1 1 or 12 for carrying out a method according to at least one of the method claims 1 to 1 1, characterized in that the output of the mill (2) is connected to a condenser (8) for cooling the mass flow, and that of Capacitor (8) has at least one input branch (9) via which additives (30) are supplied.

14. The apparatus according to claim 13, characterized in that the

Capacitor (8) is designed as a spray dryer or as a stirrer with flotation (Figure 10).

15. The apparatus of claim 13 or 14, characterized in that the output of the capacitor (8) is connected to the input of a screw conveyor (13) or other longitudinal conveyor.

1 6. Apparatus according to claim 15, characterized in that the

Output of the screw conveyor (13) with the input of an extruder (17) is connected, in the further additives (20) are supplied.

17. The device according to claim 1 6, characterized in that on

Output of the extruder (17) are connected to a device for granulation (25) or to design a different shape and a downstream device for drying (26).

18. Device according to one of claims 1 1 to 17, characterized in that the extruder (17) has an output branch (21) for the discharge of exhaust gases (23) is connected.

19. Device according to one of claims 1 1 to 18, characterized in that following the condensation stage (33) takes place a Verperlung (41), but only with supply of steam (38).

20. The apparatus according to claim 19, characterized in that on

Exit the Verperlung (41) is connected to a drying stage (42), and the in the Verperlung (41) introduced steam (44) is removed.

21. Device according to one of claims 1 1 to 20, characterized in that the additive (30) in the condensation stage (33) is admixed.

22. Device according to one of claims 1 1 to 21, characterized in that the Verperlung (41) and the drying (42) by a

Extrusion stage (34) are replaced.

23. Device according to one of claims 1 1 to 22, characterized in that in the grinding stage (32), the carbon black (29) and steam (38) are introduced.

24. Device according to one of claims 1 1 to 23, characterized in that in the extrusion stage (34) additives (31) are introduced.

25. Pre-compound prepared according to at least one of the process steps 1 to 1 0, characterized in that the pre-compound produced has the composition of a pourable granules having a particle size of about 3 mm.

26. Device according to one of claims 1 1 to 25, characterized in that at the extruder (17) via the output branch (21) water vapor is withdrawn and the heat of vaporization of the water for cooling in the extruder (17) contributes.

27. Device according to one of claims 1 1 to 26, characterized in that a part of the suspension (74) obtained at the outlet (79) is filled via a cooler in the condenser (71).