Classifications

• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
  • C10B7/00—Coke ovens with mechanical conveying means for the raw material inside the oven
  • C10B7/10—Coke ovens with mechanical conveying means for the raw material inside the oven with conveyor-screws
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
  • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
  • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E50/00—Technologies for the production of fuel of non-fossil origin
  • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

• the present invention relates to a new process for pyrolyzing wood, namely strictly speaking structured wood such as trunks or hard parts of the heart of wood and of alburnum, or of biomass, in the form of leaf residues and thin branches, remains of treated vegetable matter (sugar cane bagasse, rice straw, bran in general) or pasture or grass, this process also extending to mineral coal, after thermomechanical treatment in special ceramic retorts or metallic, in which the material is heated and simultaneously compressed continuously by means of pistons (intermittent pressure) or by means of feed screws (continuous pressure).
• the final product of the process mentioned here will be "vegetable charcoal” or “coke”, the shape of which can be chosen with rectangular or round sections, or according to the diagram appended in the form of bored ceramic products or products of full section , and the density in the form of dense charcoal (apparent density of 0.7 to 1.4) or of light charcoal (apparent density of 0.4 to 0.7) of lower or higher volatile products capable of leading to vegetable coke , with the consequent change in reactivity, also offering the possibility of choosing medium dimensions (variation from 1.0 cm to 15.0 cm, depending on what is desired). Either split charcoal or powdered charcoal can be obtained with lower or higher reactivity.
• By-products in liquid form more oxidized (acid fraction) and hydroxylated compounds (alcohol and aldehydes) if less oxidized products (with benzene, naphthenic and anthracene nuclei) can be used during the process, so as to save fuel, or add to the raw material itself, and gaseous by-products (gases and vapors) can be used during the development of the process as fuel to heat retorts, or else be sold.
• the originality of the carbo-chemical method of the present invention consists in shaping the product, by causing mechanical pressure to act on the still hot material, during pyrolysis, in using at the same time the metal retort as reactor and pressure device, or briquetting device, with a reduced loss of mechanical energy, since advantage is taken of the plastic phase, with a resistance lower than the deformation opposed by the material used.
• the invention relates to a method for manufacturing interesting carbon products, in which at least one compound chosen from forest products, derivatives of forest products and wood, materials constituting biomass, wood derivatives, cellulosic products and mineral carbon materials and derivatives, is treated as follows:
• the raw material is reduced to particles to the desired particle size.
• the mixture thus obtained is introduced into a closed distillation and forming device, while being subjected to mechanical pressure.
• the mixture is subjected inside this closed distillation device to a pyrolysis and plasticization process, after which the gaseous and liquid fractions produced during the pyrolysis process are recovered from the plasticized mixture.
• the plasticized carbonaceous fraction thus obtained is formed into a thermally interesting finished product, while being cooled in the absence of an oxidizing medium.
• the temperature, pressure and time conditions are chosen so as to obtain products chosen from dense carbon products, pulverulent carbon products, coked products, gaseous fractions and / or liquids are burned to provide heat for the pyrolysis process; the method is implemented continuously or discontinuously; the raw material has been pre-dried; the carbon product obtained according to the above method at a temperature of 300 ° C is subjected to a degassing process at a temperature rising to 900 ° C to obtain a coked product.
• the present invention also relates to a device for distillation in a closed vessel and for forming for the production of interesting carbon products, starting from at least one compound chosen from forest products, derivatives of.
• forest and wood products constituent materials of biomass, woody derivatives, cellulosic products and mineral carbonaceous materials and derivatives, characterized by the fact that it comprises: - Means for reducing the starting material into particles in order to obtain a mixture having the desired size of the unit elements or particles;
• pressure means for transferring the mixture thus ground under pressure into:
• At least one cooling device for obtaining a drop in temperature of said mixture and of the articles in the absence of an oxidizing medium.
• the reduction means at the particulate stage of the mixture are chosen from sieves, mechanical separators, pneumatic separators, for example of the cyclone type;
• the closed-cup distillation means comprise at least one ceramic and / or metallic reactor retort, which is cylindrical with a frustoconical end zone, the latter mainly forming the plasticization region of the retort;
• the heating means consist of an electrical resistance surrounding the retort;
• the plasticizing region is provided with a number of openings for discharging the gas fractions upwards and the liquid fractions or condensates downwards;
• the forming means are in the form of a tube and associated with cutting means.
• raw materials are used primary plants (trees, bushes or plants of low growth, pastures or aguapes) or secondary raw materials (industrial residues, bagasse, rice straw and remains); mineral coal can also be used as a raw material, exclusively or mixed with plant materials.
• Particle reduction of the raw material as a first step is desirable to facilitate handling and increased efficiency, but is not essential to the process, which involves using different types of equipment, such as for example saws, cutting screws, blades of various types applied to the wood industry, to reduce the raw vegetable material to more or less uniform dimensions. Wood cut into parts can also be used, the only restriction being the diameter of the reactor (a maximum of 15 centimeters).
• the crushed material is then chosen according to its size, by separation into two or more than two fractions: that intended to supply the pyrolysis reactors (furnace) - processing equipment - and that intended to be burned as fuel. This combustible fraction is low in the case of fluidized bed ovens or large in the case of high ovens.
• the selection of the particle size is made by means of sieves or other mechanical separators or by means of pneumatic separators (cyclones or others).
• the system for the continuous feeding of the mechanically prepared raw material in terms of particle size, after reduction to particles and plasticization according to the size, provides a constant pressure on the material intended to be condensed, as it progresses along the reactor (usually a metal cylinder).
• This feeding system is constituted by a mechanical or mechanical-hydraulic device, intermittent but producing a progressive movement of the material inside the reactor, or even, by means of a device of the feeder type in the die, really continuous.
• the pressure pyrolysis reaction is carried out in a metallic or ceramic (special) reactor, with good thermal conductivity, manufactured for example in carborandum.
• the pressure on the material inside the tubular reactor or the like comes from the system. mechanical supply in the external part of the reactor.
• the critical phase of the process is that in which the material reaches a degree of great plasticity, and therefore its deformation under relatively moderate pressures, relatively low compared to those corresponding to the limit of mechanical strength of the wood.
• This plastic phase is reached in a temperature range above 400 ° C, but dependent, to a large extent, on the thermal ratio of the material.
• the control program (temperature, pressure and time), for the entire operation, determines the thermal profile of the reactor which, in interaction with the geometric longitudinal profile, results in a pressure in mechanical terms, on the material put eh work (biomass associated or not with mineral coal). Consequently, the feed rate regulates the reaction time.
• pulverized carbon produced with a longer reaction time in relation to the other parameters, consisting of particles less than 100 microns.
• Light reactive carbon produced at lower temperatures, in relation to other parameters. It consists of blocks with a density of less than 0.7, the softening of the biomass in the plastic zone is associated with a certain emission of gas and vapor, which requires details of the design of the reactor, that is to solve the problem of development of high internal pressures in the charge, in order to improve the own charge flow pressure which is used.
• An example is given in Figure 2 attached.
• Heating along the reactor can be provided either by the combustion of liquid or gaseous fuels produced in the implementation itself or by means of electric heating.
• Cooling in the end region of the reactor is achieved by means of air or water circulation, and can be terminated outside the reactor, for example, by means of cooled combustible gases.
• the product, coal or coke, is collected in a special container, thus avoiding, when it is still hot, contact with air, so as to prevent its oxidation.
• FIG. 1 is a block diagram illustrating the method of distillation in a closed vessel and of forming according to the invention
• Figure 2 is a schematic sectional view of a closed distillation and forming device according to the invention
• FIG. 3 is a diagram illustrating the variation in density of the briquettes in relation to the size of the particles used in the method of the invention
• FIG. 4 illustrates the thermal profile of the closed-distillation and forming device according to the invention, at an operating temperature of 300 ° C
• FIG. 5 illustrates the thermal profile of the closed-distillation and forming device, at a temperature of 760 ° C;
• Figure 6 is an axial sectional view of a dis positive test for the implementation of a pyrolysis under pressure according to the invention.
• the continuous feed system subjects the material to a constant pressure, which becomes denser as it progresses inside the reactor (usually a metal cylinder).
• the feed system consists of an intermittent mechanical or hydromechanical device, which produces a gradual movement of the material inside the reactor, or otherwise, by means of a device of the "screw feed" type, which is effectively continued.
• FIG. 2 of the drawings there is shown an example of the reactor studied, in the case of obtaining a "reactive light coal", where a design detail is presented, for a reactor where there are three zones reaction: the heating zone, before the plastic zone, where a low temperature prevails; the plastic zone where the condensation of coal takes place, with a simultaneous separation of the fractions of the fluid (liquid and gas); the overheating zone, necessary only in the case of the products of steps 5 and 6, and the cooling zone.
• the reactor is heated by the use of liquid or gaseous fuels produced during the operation itself, or otherwise, by electrical energy.
• the heating of the extreme zone of the reactor is carried out by circulation of air or water, and can be carried out outside the reactor by means of the gases of the cold fuel.
• the final product - coal or coke is put in a special container, contact with air being avoided while it is hot, so as to avoid its oxidation.
• the continuous process of carbonization with shaping can be applied for carbonization and / or "coking" made continuously, and can also be adapted for batch operation, when it is used on a small scale; in this case, the program necessary for the feeding time is made, in cycles.
• the program necessary for the feeding time is made, in cycles.
• this aspect is relevant, since the investment and the costs of real estate associated with a briquette formation unit play an important role in, the composition of the final price of the shaped product (coke) or briquettes made of vegetable charcoal, produced according to conventional methods.
• charcoal obtained experimentally either from biomass (branches and leaves), or tree trunks, is present at a density of about 1.0 - more than double the average density of vegetable charcoal current - favorable element for the economic aspect of the transport of the product mass per unit of volume available larger for transport.
• the process for manufacturing precious carbonaceous materials has a main characteristic: the interaction between two unit operations, always carried out outside the classic technique now used: carbonization of biomass, during pyrolysis and / or the transformation of mineral coal into coke, on the one hand, and mechanical formation, on the other hand, thus making it possible to obtain solid products having different reactivities and densities, from coals light reagents up to dense coke with low reactivity, in dimensions ranging from blocks of 15 cm (coal or coke formed) to finely pulverized carbon, with a particle size of less than 100 microns.
• Tables 1 and 2 in conjunction with Figure 3, list the characteristics that are important as a parameter for processing. adopted for biomass, following specific tests carried out, for the formation of briquettes by compression (pressure adopted after attempts ; 39 x 10 4 Pa).
• Figures 4 and 5 show the control of the thermal level, taking into account the geometry of the retort used, made of heat-resistant steel (AISI 302).
• FIG. 6 This device comprises a support cylinder 3 mounted in a body 2 of an oven made of insulating refractory material 13.
• a support cylinder 3 mounted in a body 2 of an oven made of insulating refractory material 13.
• a outer cylinder 5 with a half-cone 4 so as to form the limits of a retort 6, the arrangement being surrounded by a resistor 7.
• a compression piston 12 cooperates with a pressure screw so as to apply pressure to the inside the cylinder 5.
• the cylinder 3 has flanges 1.8 at each of its ends.
• a bearing with thread 11 for the passage of the piston rod 12 is fixed to the flange 8.
• a tightening measuring device 10 a temperature gauge 14 and a condenser 15.
• the biomass is gradually compressed during the pyrolysis process. Excellent results were obtained in examining the characteristics of the residual fuel after pyrolysis, and the result was that a homogeneous, dense, resistant structure of the precious carbon product was thus obtained.
• the pre-dried pulverized mixture is introduced along the arrow f1 via a hopper 21 into a retort 22 in which the mixer is mechanically compressed by a feed screw 23 driven by an outer shaft 24 actuated by a motor means (not shown in the figure).
• the hopper 22 is surrounded by a dispo heating sitive 25 and comprises a cylindrical zone in which is mounted the feed screw 23 and a frustoconical zone 22b directed upwards which is formed so as to allow the gases produced during the process of pyrolysis to escape and directed towards bottom so as to allow the liquid condensed in the retort to flow, while preventing the discharge of the plasticized mixture.
• the frustoconical plasticization zone 22b is connected to an extrusion tube 26 to allow the exit of a shaped mixture which can then be cut to the desired size.
• the frustoconical zone 22b, the extrusion tube 26 and the respective discharge pipes 27, 28 of the gases and of the condensate are surrounded by a jacket of cooling water 29.
• the extruded mixture which is a carbonaceous product, is then cooled in a chamber (not shown in the drawings) which is free from any oxidation medium.
• the densified carbon obtained under a temperature of 320 ° C. is degassed under pressure, at a temperature of 900 ° C.
• the complete operation lasts from 120 to 150 minutes.
• the vegetable coke obtained in compact form has mechanical and chemical properties which are satisfactory in terms of industrial use.
• Table 8 summarizes the analytical results and properties.
• liquid condensate obtained in pyrolysis gives the following values on average per 100 grams of dry biomass:
• the condensate contained a high amount of water, the non-aqueous part consisting mainly of phenol and methyl alcohol (49.8%) plus volatile acids (22.1%) and the rest comprising hydrocarbons, mainly belonging to the aromatic series.
• the gases produced in the eucalyptus pyrolysis gave the following analysis results at low temperature (320 ° C);
• the method of the present invention has the following advantages: 1) It is a process of carbonization or continuous transformation into coke, which can also be adapted to non-continuous methods ( in batches), in the case of a small-scale operation.
• the programming of pressure and time is made by operating cycles or residence time, in the case of the continuous process.
• the process of the present invention combines, in a simple operation, the pyrolysis of biomass (plant material) or the transformation of mineral coal into coke, with the mechanical formation of the product, thereby exempting the operation of formation in coal or coke briquettes.
• This aspect is relevant, since the operating costs and the investment of the briquette training unit are very important in the composition of the price of the product - coke or briquettes of charcoal considered economically.
• FIG. 10 highlights the difference between the conventional method and the new method, and one can see the great simplification obtained.
• the process of the present invention presents flexibility in the production of combustible products, with variable dimensions, from blocks of 15 cm in dimensions - coal or coke formed - to finely divided coal, with lower grains at 100 microns or 0.1 mm.
• the process of the present invention is suitable for treatment (change to coke or pyrolysis) either for plant biomass or wood, or for mineral coal or a pulverized mixture of the two, which is of great interest.
• the process of the present invention has as main characteristic the interaction between two unit operations, always separate, in the current industrial technique: the carbonization of biomass, by pyrolysis, and the change of mineral coal into coke, and the formation mechanical on the other hand.
• This interaction of the heat treatment with the mechanical formation of briquettes is combined in optimum terms with a control that can be made automatic by 3 or more variables (pressure, temperature and speed or time), using the existing plastic phase, as we know, in mineral coal, and now found in plant biomass.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Materials Engineering (AREA)
• Organic Chemistry (AREA)
• Solid Fuels And Fuel-Associated Substances (AREA)
• Processing Of Solid Wastes (AREA)

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• 1982
  • 1982-11-12 JP JP57503393A patent/JPS58501912A/ja active Pending
  • 1982-11-12 EP EP82903322A patent/EP0093136A1/fr not_active Withdrawn
  • 1982-11-12 WO PCT/FR1982/000187 patent/WO1983001781A1/en not_active Application Discontinuation

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