DE2234755C3 - Process for the production and recovery of chemicals and fuels from waste containing organic solids, in particular waste - Google Patents

Description

The invention relates to a method for producing and recovering chemicals and fuels from waste containing organic solids, in particular garbage.

The removal and destruction of solid materials generated as waste in industry and households, which are referred to as garbage in the following description is growing into a formidable problem. The costs of this public service are e.g. B. in the United States of America in public Household currently in third place behind the school system and road construction. The cost per unit in waste disposal and the number of units of waste generated per person are increasing every year Year. It is estimated that each individual

for example in the United States of America generates 4 to 6 pounds of garbage per day and that garbage production industry is about 5 pounds of solids per person per day. The cost of garbage disposal vary between 12 and 75 DM per ton of waste. The known procedures waste disposal, such as rubbish dumps, are therefore increasingly no longer feasible, while other processes, such as waste incineration, are downright expensive and too Air pollution problems. It is therefore imperative to be able to work effectively To create facilities and means for the destruction of solid waste.

A second aspect of this problem is that the woes use their natural stores constantly increasing speed consumed. In the normal cycle when using Materials, the raw materials are obtained, processed into useful products, by the consurants different periods of time are used and then hardly usable again Hand over wasteland, namely the urban garbage dump.

The increasing shortage of raw materials has already led to various proposals to recover valuable components from waste. For example Aluminum and glass manufacturers buy used tin cans and bottles for reprocessing. Engineering studies and plant designs are already in preparation, around the basic concept of using the heat generated by waste incineration for To further develop the operation of electricity generation plants and desalination plants.

The recovery of metallic constituents from garbage has long been in this area of technology Known for a long time and forms an integral part of the steel industry.

However, since the non-metallic constituents of the garbage form a large proportion therein, it is now necessary that the art develop methods which allow both the metallic and the non-metallic constituents of the garbage to be recovered as raw materials. The simple incineration of the organic part of the waste to generate usable heat is not the optimal solution for many reasons. The exhaust gases generated during the incineration contain substances that pollute the air, such as SO ₂ , NO ₁ . CO and ashes. These poisons and impurities must be captured or rendered harmless, which requires extremely expensive systems such as electrostatic separators, washing systems, etc., in order to avoid the risk of air pollution. In addition, organic solids in waste are a poor fuel and cause very high combustion temperatures. There is, therefore, a significant need for a truly effective, economical method of treating the common waste generated by society today, by means of which the levels of chemicals and fuels can be recovered from both the inorganic and organic parts of the waste, while the volume quantities of gaseous products to be subjected to separate treatment to avoid air pollution must be reduced significantly at the same time.

A significant amount of discarded raw materials is currently being recycled by many companies \ v economics, soft in the field of Secondary material industry. Large amounts of metals, a significant amount of paper and a Part of the glass is collected, processed and reused. With the exception of tinplate and However, aluminum cans in a few areas become only a small proportion of those that are reusable Amounts of raw materials recovered in the US after being once in the stream of the public Garbage collection have been received. A typical breakdown of urban waste is as follows Table 1 summarized, and the most difficult problem here is the immense amount to separate contaminated and spoiled materials from this heterogeneous mass and the recover potential values shown in the table below.

Table 1

Recyclable materials in municipal waste

Raw material Together
settlement
(Weight
percent) Dear one
Efficiency
the again
extraction
(Vo) Group 1 Magnetic Metals
Non-magnetic
Metals
Glass
Dirt and debris
Subtotal 6 to 8
1 to 2
6 to 10
2 to 4 95
95
80
0 Group 2 Paper products 48 to 55 50 Group 3 Not again- ~ 55
recovered paper and
other organic
Fabrics 100

The invention is concerned with solving the above problems, and in particular has The task set to create a method of the type mentioned above, through which the previously not recyclable organic components of urban and industrial waste valuable chemical compounds can be won.

This object is achieved according to the invention in a method for the production and recovery of chemicals and fuels from waste containing organic solids, in particular garbage, in that a ^{particulate waste material containing less than 10 0} / o organic substances and hot particulate animal and bone charcoal with a relative of the waste material inert carrier gas is combined into a gaseous stream and the gaseous stream is passed with turbulent flow in a pyrolysis zone for a dwell time between 0.05 and 10 seconds, in this case the waste

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Fall material is heated to a temperature in the range between 150 and 1400 ⁰ C and that the organic chemicals and fuels are removed from the pyrolysis zone or that the particulate animal or bone coal and the organic chemicals and fuels together from the Pyrolysis zone are removed and that the animal or bone coal is then separated from the chemicals and fuels, and optionally a part of the solids removed from the pyrolysis zone is heated and returned to the circuit to form the turbulent gaseous flow.

In the method according to the invention, the particulate waste material is by heat exchange in heated for a very short period of time, the heat transfer medium being the "animal or bone charcoal" designated coke product of the process itself is used and wherein the particulate waste material and the hot particulate heat carrier both in the form of a turbulent gas flow in a fast moving inert carrier gas. The speed of the pyrolysis process, d. H. the rate at which the waste material heats up to the pyrolysis temperature is of particular importance in order to achieve the success aimed at according to the invention, namely, from this waste material useful organic chemical compounds and fuels to win. If the heating of the waste to the required pyrolysis temperature takes a longer period of time would require completely different pyrolysis products would arise, in particular the inorganic chemical compounds and fuels released during heating, at the same time be degraded before the heating is finished. The nature of the process of the invention is thus such that its success depends on operation under very special conditions, so that the different reaction rates occurring at the different with each other competing chemical reactions that occur during and after heating the waste material the specified high temperatures run, can be used in an advantageous manner to achieve the desired manufacture valuable pyrolysis products.

However, the required high speed of heating can only be achieved in that ensures extremely rapid heat transfer from a heat transfer medium to the waste material will. A fluidized bed reactor, as it is known for example from DT-PS 9 50 317, is for this Purposes in any case not suitable, since the use of such a reactor type is comparatively long Residence times of the waste material would result, so that the relatively rapid degradation reactions of the products make the production more valuable Pyrolysis products were prevented. In addition, the method described in DT-PS 9 50 317 is used using a fluidized bed reactor of the simultaneous generation of strong gas and Lean gas from solid fuels, which are almost homogeneous compared to municipal waste.

From DT-PS 9 74 376 there is also a method and a device for degassing dusty or fine-grain fuels are known which are also compared to municipal waste homogeneous fuels. In addition, the principle applies with regard to the degassing speed same as in the method known from DT-PS 9 50 317, since here the degassing in one Mixing screw is made in which the heat transfer medium and the fine-grain fuel are intimately connected are mixed, which necessarily take place at a comparatively low speed got to. In this known process, the heat is transferred directly between the solids and not when the solids are in suspension in a turbulent gas flow. In contrast, the Method according to the invention, the heat exchange is therefore carried out within a turbulent gas flow so that the heat exchange between the solids without heat loss at external device parts can be done to thereby achieve the aforementioned rapid and effective heat transfer to enable.

In the DT-AS 11 35 419 a method is also described in which a fine-grained carbonaceous Heat transfer medium externally heated by fuel gases and then with a to be heated Material is mixed while the heat carrier and the material are swirled in a flow of conveying gas will. Any limitations on the residence times of the individual substances are known in this case Procedure not addressed.

The inventive method has the particular advantage that the previously unusable organic content of waste in clean-burning heating fuel with a low sulfur content can be converted using more than 1.6 hl of good quality liquid heating fuel per

Have one ton of wet urban waste obtained in the condition in which it was delivered. Regarding the details and the For many other advantages, reference is made to the examples below.

In detail, the invention can be further-

are formed so that the organic chemicals and fuels discharged from the pyrolysis zone rapidly cooled to a temperature below the pyrolysis temperature. This creates the danger a degradation of the valuable process products

decreased.

An advantageous embodiment of the invention can be created in that the residence time of the waste material in the pyrolysis zone is maintained for less than about 1 second.

A preferred temperature range of the waste material in the pyrolysis zone is between 315 and 665 ° C.

According to a preferred embodiment of the invention, before heating in the pyrolysis zone

the inorganic contained in the waste material Substances are essentially completely separated. In detail, the method according to the invention be carried out so that the particle size of the waste material is maximized is brought less than 2.5 cm.

In a particularly preferred embodiment according to the invention, the separated, in the circuit returned animal or bone charcoal is previously heated to a temperature between 620 and 980 ° C. A particularly preferred embodiment according to the invention can be created in that a quantity of carrier gas with the particulate waste material and the hot particulate animal

or charcoal is combined, which is sufficient to generate a turbulent gas flow with a Reynolds' Form number of at least 2000.

In detail, the invention can be further developed in that the weight ratio of Carrier gas to particulate! Waste material between 0.2: 1 and about 2: 1 in the turbulent gaseous Current is set.

It is preferred here to heat the particulate waste material in the pyrolysis zone to a temperature between 150 and 815 ^{° C. by controlling the amount of particulate animal or bone charcoal.}

In this procedure it is advantageous to reduce the weight ratio of hot particulate animal or charcoal to particulate! Waste material in the turbulent gas stream to at least 2: 1 to adjust.

In the method according to the invention, it can also be advantageous in particular to use a carrier gas to use hydrogen-enriched gas stream.

An advantageous embodiment of the invention is characterized in that as waste material solid waste, in particular municipal waste, manure, sewage sludge, automobile tires, untreated process waste, Agricultural waste, industrial waste, tree bark, rice husks or mixtures of these Substances, is used.

To improve the heat balance, it is also advantageous to adjust the waste material to a moisture content of less than 5 percent by weight.

The invention also provides a liquid organic compound and fuel obtained from a waste material containing organic solids, in which the particulate waste material containing less than 10 ⁰ O inorganic substances has been combined with hot particulate animal or bone char and a carrier gas , which is substantially non-oxidizing with respect to the waste material to form a turbulent gaseous stream, the turbulent gaseous stream being passed into a pyrolysis zone for a residence time between 0.05 and about 10 seconds in which the waste material to form liquefiable organic chemicals Compounds and fuels was heated to a temperature between 150 and 1400 ° C by appropriate choice of the temperature of the particulate animal or bone charcoal in the pyrolysis zone and the chemical compounds and fuels were condensed.

The method according to the invention is based on the heating of particulate, for example shredded organic waste materials in the absence of air using a new heat exchange system. Experiments on a laboratory scale and on test facilities lead to organic yields Chemicals and liquid fuels in excess of 40 percent by weight that are produced from oven-dried, Input materials free of inorganic substances were achieved. The liquid fuel has has an average calorific value of about 6700 kcal / kg and can be used as a substitute for a No. 6 heating oil with low sulfur content can be used.

The pyrolysis of organic waste continues to produce animal or bone char, gases and a fraction of water. The distribution of these products represents the. most important economic factor in relation to commercial Most of the systems known from the prior art produce comparatively little organic liquids unless high pressure hydrogenation is used. A Example of the distribution and analysis of the products that can be achieved by means of the method according to the invention are summarized in Table 2 below

Table 2

Pyrolysis products

Animal or bone charcoal, 20 percent by weight;

Calorific value 5000 kcal / kg

48.8 weight percent carbon
3.9 percent by weight hydrogen
1.1 weight percent nitrogen
0.3 weight percent sulfur

31.8 weight percent ash
0.2 percent by weight CMor

13.9 weight percent oxygen (difference)

Oil fraction, 40 percent by weight;
Calorific value 6700 kcal / kg

57.5 weight percent carbon

7.6 weight percent hydrogen

0.9 weight percent nitrogen

0.1 weight percent sulfur

0.3 weight percent ash

0.3 weight percent chlorine

33.3 percent by weight oxygen (difference)

Gas fraction, 27 percent by weight;
Calorific value 53.4 kcal / m ³

0.1 mole percent water
42.0 mole percent carbon monoxide
27.0 mole percent carbon dioxide
10.5 mole percent hydrogen
<0.1 mole percent methyl chloride

5.9 mole percent methane

4.5 mole percent ethane

8.9 mole percent of C ₃ to C. hydrocarbons

Water fraction, 13 weight percent

Contains:

acetaldehyde

acetone

Formic acid

Furfural

Methanol

Methylfurfurol

phenol

etc.

In addition to the 40 percent by weight organic liquid fuel yield that is typical for a Run is achieved, about 20% animal or bone char, 27% gases and 13% Creates water. The gases and part of the animal or bone charcoal are used as a heat source to carry out of the process, and the organic liquid and the remaining animal or bone charcoal can be sold as fuel or raw chemical will

609 034/186

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material and hot particulate animal or bone charcoal. The choice of a particular temperature, however, will depend on the particular waste organic solids being used and the residence time of the waste solids in the pyrolysis zone. The gaseous stream is in a pyrolysis zone for a period of time which is generally less than 10 seconds, preferably about 0.1 to about 0.6 seconds. In general, it has been found that organic solid waste from municipal waste sources can advantageously be treated by means of the process of the invention by heating the organic waste solids to a temperature in the range between about 425 and about 540 ^° C in the pyrolysis zone, the residence time being between 0 , 1 and 2 seconds. When the process is conducted such that the organic solids are heated to a temperature of about 485 C in the pyrolysis zone, a residence time of about 0.3 to about 1.3 seconds is preferred. If wastes containing at least 70 ° ο cellulosic materials are used, a temperature between about 425 and about 455 ° C is preferably used with a residence time of about 1 second or less. When treating automotive tire particulate waste, lower temperatures, for example between about 150 and about 260 "C, may be used. The relationship between temperature and residence time can be varied to optimize the yields of liquid organic chemicals and fuels. If If the temperature and / or residence times are too low, the evaporation and pyrolysis of the organic solids of the waste material is incomplete, and if the temperature and / or residence times are too great, the pyrolysis products will degrade and result in low yields of liquid chemicals and fuels.

The expression "turbulent flow" denotes a gas flow flowing through a pyrolysis zone, for example a tubular reaction vessel where the flow is turbulent in nature, d. H. has a Reynolds number greater than 2000, and preferably about 2500.

In operation, only a low ratio of about 0.2 to about 2.0 pounds is more mixed Gases per pound of solid waste required to have a Reynolds number of 2000 or greater, when the pyrolysis chamber has a diameter of 76 mm or more. For example with a Only 0.7 pounds of gas per pound of solids are required to produce chambers with a diameter of 254 mm maintain a turbulent flow in the chamber. Laminar flow in the pyrolysis zone must be avoided as such a flow system tends to significantly reduce productivity and limit the rate of heat transfer within the pyrolysis zone. In the normal practice of the invention are the carrier gas, the hot animal or bone char and the solid waste is introduced into one end of a pyrolysis vessel and rapidly mixed together and dynamically brought into contact with each other as they are blown through the vessel to allow the required heat transfer to take place.

Those for the thermal decomposition of the organic substances and for the removal of the volatile organic substances Heat required by chemicals can be partially or completely due to the sensible warmth of the hot animal carbon particles are supplied, but preferably substantially all of the heat delivered by the hot animal charcoal. From about 2 pounds to about 10 pounds of hot animal charcoal preferably used per pound of solid waste. The use of hot animal charcoal as a heat source in the pyrolysis zone has many advantages. Due to their heat capacity and density, one is essential less volume of animal charcoal is required to heat the solid waste than is the case would be if only the hot carrier gas were used. The hot animal charcoal comes into close contact with the solid waste in the turbulent gaseous flow, thus creating a heat transfer high efficiency.

The choice of an optimal weight ratio between animal charcoal and waste materials naturally depends on the heat transfer required in the system. As part of the warmth of the Pyrolysis can be supplied by the carrier gas, the temperature, the flow rate and the Residence time in the reactor by means of those well known Procedure for the particular system can be calculated.

The thermal energy can continue to the pyrolysis zone by means of indirect means, such as electrical Heating to be fed through the zone wall.

The carrier gases that have been found to be useful in the process according to the invention to carry out the thermal elution of the solid waste particles are not those that are associated with the animal charcoal, with the organic substances and with the organic chemicals that are formed during pyrolysis react. The carrier gas stream should be essentially free of air and oxygen, the gas stream preferably containing less than 40% oxygen, ideally less than 1% oxygen. The amount of oxygen is kept as low as possible in order to keep the oxidation of organic substances including the liquid chemicals and fuels obtained as low as possible. Examples of gases suitable for use as the carrier gas are nitrogen, argon, CH ₄ , H ₂ , carbon monoxide, flue gases, carbon dioxide and any other gases that do not adversely react with or with the organic content of the substances in the system oxidize. In preferred embodiments of the invention, the carrier gas is circulated back into the pyrolysis zone after the organic chemicals have been removed therefrom.

The effluent or the exhaust gases from the pyrolysis zone consist of animal charcoal, vaporized organic Fuels and chemicals, generator gas and carrier gas. In a preferred practical mode of operation the evaporated organic fuels and chemicals are then brought to a temperature Cooled below the pyrolysis temperature to prevent the decomposition of organic chemical substances to reduce. The solids consisting of animal charcoal can easily be converted into any of the usual Solid-gas separators, such as cyclone separators or the like, for example, are separated. The Ver-

Vaporized organic chemicals and the carrier gas can be separated from each other by means of conventional separation and Recovery agents are separated and recovered.

If the waste solids that have passed through the pyrolysis zone contain inorganic materials such as metal and glass, their particles appear mixed with the animal or bone char produced by the organic fraction of the waste solids in the effluent from the pyrolysis zone, but the organic and inorganic solids can easily be separated from one another using standard air classification systems. Indeed, the pyrolysis of the organic solids increases the density difference between such solids and the inorganic solids, which in fact facilitates their separation in the effluent from the pyrolysis zone. Animal or bone carbon solids, which contain both inorganic and organic solids, can be recirculated through the pyrolysis zone to provide the required amount of heat without first being separated. However, if the solids effluent from the pyrolysis zone are separated, the heat content of the inorganic solids can be recovered in a manner to provide the heat for the pyrolysis zone to increase the efficiency and economy of the system. For example, the heat contained in the inorganic solids can be used to heat the circulating gases. Alternatively, the inorganic solids can be separated from the animal or bone char by conventional means, if desired. However, it will be apparent to those skilled in the art that hot inorganic solids recovered from the effluent of the pyrolysis zone are in excellent shape and condition for further processing by conventional methods to recover the metallic or inorganic chemical constituents therefrom. This factor further improves the economy of the process.

The generator gases produced by the pyrolysis of waste solids generally contain condensable hydrocarbons, which can be easily recovered by condensation, and non-condensable gases, such as carbon dioxide, carbon monoxide, hydrogen and methane and other hydrocarbon gases, which cannot be obtained by conventional condensation. The generator gases also contain undesirable gaseous products such as NH ₃ , HCl, H ₂ S and water, which should be removed from the generator gas flow by means of conventional devices such as cooling and chemical washing systems. After the condensable organic chemicals and undesirable gaseous products have been removed from the generator gases, the resulting gases can be used to provide the heat for the process and recycled as a carrier gas for the pyrolysis of other waste materials.

Initially, the process will be started using hot bone char from other sources but after waste solids have been pyrolyzed in the process, is left by pyrolysis more than enough hot animal charcoal is generated to keep the process complete and independent of one external source to make hot animal charcoal. Excess animal or bone charcoal can easily be used up to be processed in further treatment for the production of new materials, whereby the overall economy of the process is improved, such as as a fuel for Use in a power generation plant or as a raw material source for the chemical industry.

ίο The excess animal or bone charcoal can for example briquetted by conventional means for use such as coke.

The excess animal or bone charcoal produced by the process can also, if desired, be ^{degassed by heating to temperatures between 650 and 980 °} C. or higher in order to give off a hydrogen-rich gas which can be sold as a high-quality fuel. The gas can still be converted to pure hydrogen or upgraded, or used to hydrotreat the heavier vaporized chemicals produced by the process.

The animal or bone coal degassing can be done by direct or indirect heating. at

As the direct heating, the charcoal is in Contact with a sufficient amount of oxygen from an appropriate source such as Air, brought to the gas flow through controlled combustion to the desired degassing temperature bring to. This can be done in a transport reactor similar to the pyrolysis reactor or in a fluidized bed reactor respectively.

Preferably, however, the animal or bone charcoal is degassed by indirect heating in order to obtain a To yield gas flow that contains more than 70 or more percent by volume of hydrogen. This can be done in take place in a reactor, which is similar to a tubular heat exchanger, in which the animal or Biochar is blown through the pipes in a dense or dilute phase, with a Fuel burned with air or other appropriate source of oxygen in adjacent pipes to deliver the vat required for degassing. Alternatively, the same can be done Result can be achieved by burning a fuel in pipes that are made in a fluidized bed Animal or bone charcoal are arranged. After separating the remaining solid, degassed animal or Bone charcoal from the released gases is ultimately cooled to the animal or bone charcoal to be used as a high grade fuel.

If desired, a low sulfur animal or bone char made from waste solids Produce that contain large amounts of sulfur can reduce the sulfur during the Pyrolysis or by overheating and / or degassing the resulting char.

The desulfurization during pyrolysis can be achieved by adding a sulfur acceptor in the form a solid, such as lime or iron oxide, is present in the pyrolysis zone during pyrolysis is. The sulfur combines with iron oxide to form magnetic gravel, which is magnetic and in addition to any naturally occurring iron pyrite by magnetic separation of the generated char can be removed. This can conveniently be done with minimal cooling the charcoal of the bones in order to

the same amount of heat for recirculation or for further thermal treatment to get the charcoal.

The desulphurisation can still be achieved during the pyrolysis! be that the gas flow is enriched with hydrogen, which is preferably a part of the during a subsequent bone carbon degassing released hydrogen gas isL Hydrogen fed into the pyrolysis zone reacts with the sulfur and forms sulfur sulfite, which at a later point in time by means of the usual means, such as washing, can be removed. An addition of hydrogen to the hydrolysis zone enriches at the same time the evaporated hydrocarbons. In preferred embodiments of the invention a carrier gas is used which contains at least 20 percent by volume hydrogen on the basis of the Contains total volume of the carrier gas used.

The desulphurisation can furthermore be achieved in that the resulting animal or bone charcoal is heated in a transport gas enriched with hydrogen. This gas reacts with the Sulfur in the animal charcoal or bone char to reduce sulfur in the charcoal produced deliver. As with desulphurisation during pyrolysis, the hydrogen used can get through Recirculation of exhaust gases resulting from the degassing of the charcoal are supplied, before or after cleaning the gases.

If it is desired to reduce the sulfur content of the animal or bone charcoal produced, will this, which is already at an elevated temperature, only to about 1350 to 1550 ° C at ambient pressure in a non-oxidizing atmosphere for periods of time up to about 20 minutes heated. This leads to a considerable reduction in the sulfur content in the animal or bone charcoal.

If the carbon is degassed by indirect heating, a pressure of approximately 1.05 to 7.03 kg / cm ² and the use of a hydrogen-rich carrier gas during the degassing will help remove the sulfur. Under these conditions, the animal charcoal can be desulphurized and degassed at the same time, the reaction times being approximately 10 minutes. This desulfurization can best be achieved if the inorganic sulfur has essentially been removed by a sulfur acceptor in a preceding treatment.

A typical embodiment of the invention is illustrated schematically in the drawing.

In the drawing, there occurs a broken particulate garbage containing organic solids, or Pulp from a dewatering press (not shown) into a thermal decomposition unit a line 2, which has a feed hopper 4 as an intermediate storage. The waste material supplied is measured by a valve 6 and enters a line 8 where it is mixed with a mixture brought together from air from a fan 10 and recirculated gas from a mixing vessel 12 will. The supplied and mixed gases pass through a line 14 and are in one Dryer 16 dried if necessary or in an economical manner if possible. The dried ones Solids and gases get through a pipe

device 18 in the cyclone separator 20 to the dried Separate solids from the gases. The gases are discharged through line 74 and exit into a gas cleaning unit 72. The dried solids leave the cyclone separator 20 through a line 22 and are stored in an intermediate storage vessel 24.

The dried waste solids are then placed in a pyrolysis system indicated generally at 25

ίο metered by a valve 26 and get through a line 28 to a line 30 where it is circulated with hot gas from a line 99 are brought together. The electricity of hot gas and solid waste is used during transportation through line 30 with hot, circulating animal or bone charcoal and volatile, gases fed to line 30 through line 60 are brought together. The stream of gases Animal or bone char and introduced solids then enter a pyrolysis reactor vessel 32. In the pyrolysis reactor vessel 32, the particulate solid waste materials in this embodiment to a temperature in the range of about 260 to about 835 ° C through the bite, im Recirculated char, volatile gases, and circulating gases are heated. The organics in the waste solids are thermally decomposed in the pyrolysis reactor vessel 32 and evaporates to produce chemicals and fuels that are at the pyrolysis temperature present in vapor form to form the generator gases.

A stream of gases, animal charcoal and generator gases is drawn from the reactor vessel 32 through a conduit 34 discharged to a cyclone separator 36, in which the gases are separated from the animal charcoal and passed through a line 76 can be discharged. The gases are cooled in an extinguishing tower 78. The condensate from the quenching tower 78 leaves this through a line 80 and is by means of a pump 82 in one Pumped line 84, which leads to an oil storage vessel (not shown). The not condensed Gases from the quenching tower 78 exit through a line 86 and are in a condenser 88 continued to cool. The further cooled gases and the condensed liquids leave the Capacitor 88 through line 90 and enter phase separator 92. At this point you are three phases present, namely gas, oil and water.

The gas exits phase separator 92 through line 93 and is circulated for recycle compressed in a compressor 95. The compressed gases are in the pyrolysis system of the Compressor 95 returned through line 97, preferably after heating. Part of the compressed Gases is fed directly into the pyrolysis reactor 32 through line 99 and line 30 in the above fed in the manner described. The remaining compressed gases are fed into the mixing vessel 12 sent and used to dry the fed waste material in the manner previously described. Additional fuel or other waste heat can be used for this drying step can also be used.

The water from the phase separator 92 is discharged through line 94 and through a pump: 96 pumped into a line 98 in order to use conventional devices and means in a wastewater treatment

609 634/186

Appropriate procedures are used. For example, urban waste contains between 70 and 90 «.Ό cellulosic Substances and creates a new oil by the method according to the invention.

For the purpose of description, the term "cellulosic material" is used to denote a material which contains cellulose or cellulose derived products. Typical cellulosic fabrics Include the following materials: paper, tree garbage i

Appendix 100 to be processed. The water is then drained after treatment in a conventional manner. A portion of the separated water is also circulated back into the quenching tower 78 as a coolant. The oil from the phase separator 92 is discharged through a line 102 and by means of a pump 104 through a line 106 to the line 84 and consequently to the oil storage

^ge D? e ^? e ™ or charcoal from the pyrolysis i «. Bark, sawdust, vegetable waste, such as, for example , reactor vessel 32 , sugar cane leached out after the separation described, leached sugar from the gases in the cyclone separating beet, rice husks, carrot-topped fruit, through a line 38 to animal shells, fruit kernel housing, tree waste, leaves carbon pick-up 40 removed. Part of the animal charcoal and the like. Up to 40% and in some cases up to is used to supply the process heat, 15 to 85 · .Ό of that by means of the process from waste and part of the animal charcoal is through a distribution material which is not less than 70 weight pro valve 42 from the coal pickup 40 and via a cent cellulosic or cellulosic materials ent-measuring valve 42 o in a line 44 passed. This behavior, produced oil is soluble in water. This oil driving animal charcoal is brought together with combustion air from is comparatively insoluble in non-polar solutions of a blower 46 and a line 47, such as carbon tetrachloride, and is brought into an animal charcoal heater 48 via a heptane and decane. The oil contains fed between unge-line49. A portion of the animal charcoal is burned about 10 and about 15% titable carboxyl in the animal charcoal warmer 48 to remove the acids, the acids having a pH _a of about 4.5 including the temperature of the animal charcoal at about 870.degree. The viscosity of the oil has to be increased considerably. The heated animal charcoal of the 25 is higher than that of a No. 6 heating oil. The oil is conducted both animal charcoal heater 48 through a line 50 to an acetone and other organic polar cyclone separator 52, where the fuel gases are separated from solvents such as methanol, hot animal charcoal. The Brenn- no] and ethylene glycol, soluble. The oil has a gases are discharged through a line 53 and with a comparatively high pH value of between and hot compressed gas in the line 97 30 hazards 1 and 3. The oil, more commonly combined to be used to dry the waste from about 10 to about 20% water, material in the drying vessel 16 in the manner described by those skilled in the art. familiar distillation or extraction processes

The hot animal charcoal can be removed from the cyclone separator 52. The oil contains small amounts

is through a line 54 into a memory 56 for 35 (less than 5%) of the following compounds: Acet-

the hot animal charcoal is discharged, from where it is converted into the aldehyde, acrolein, furfural, 5-methyl-2-furfural

Pyrolysis system 25 through a valve 58 and the dehyd, pyruvaldehyde, phenol, acetol, furfuryl alcohol

Line 30 leading line 60 is metered. hol, methyl ethyl ketone, acetone, cyclohexanone, 2-Hy-

The animal charcoal from the charcoal collector 40, hydroxy-3-methyl-2-cyclopenlen-1-one, acetic acid which is not used for process heat, 40 formic acid, glycolic acid, lactic acid, dimilk is passed through valve 42 to a measuring valve 426 acid, methyl formate and 2-methylfuran. It is directed and arrives in the line 48. This animal is taken that the largest constituent of a chemical charcoal is mixed with the single component of the oil levogleucosan water produced by the process from a line 62, whereby itself and other decomposition products, such as the water converted into steam, which entrains the hot 45 5- (hydroxymethyl) -furfuraldehyde, glucofuranose animal charcoal and they are in a cyclone separator and glucopyranose, which by separating the 64 carries. The resulting steam (with
Pressure of 150 psi) is released from the cyclone separator
64 discharged through line 70 and to the gas

1,4-glycosidine members of cellulose with a subsequent intramolecular rearrangement of the monomer units. Obviously

cleaning unit 72 forwarded. The hot animal 50 acts by heating the hydroxyl groups of the

Coal from the cyclone separator 64 enters a storage vessel 66 for produced animal coal and is directed to a press or the like (not shown) through a valve 67 and a conduit 68.
Wi bb

During pyrolysis, cellulose substances decompose these groups to form caboxyl groups, which causes the resulting oil becomes soluble in alkali and a number of color changes of the resulting oil from

As indicated above, the waste materials include yellow, reddish brown, and finally black rialien, which is effected by means of the method according to the invention. Everything so far from waste materials, rens can be treated, typical municipal waste, industrial waste such as tree bark,

Rubber waste, rubber powder, old rubber tires,

The ^{oil produced containing 70 0} O or more cellulosic materials was dark reddish-brown in color and is quite soluble in alkali. Did-

ground tire carcasses, waste of sugar - the thing is that a dilute solution of alkaline soda Refineries, corn on the cob, rice husks, animal substances prove to be ideal solvents for removing the from slaughterhouses or processing plants, oils from surfaces, clothing and the skin - sawdust and the oily waste one that has issued from.

Ships are incurred when cleaning their tanks. The elementary analysis of the

Stadtmüil and the waste of vegetable or natural processes from waste ^{materials that contain organic ^ 1} vegetable raw materials contain more than 70% substances, manufactured oils, such as ¹ cellulosic substances and produce a characteristic from rubber tires, tree bark or cellulose-like oil when used as a use for the inventive material, shows that the oil from the following in Ge "

AL -

The weight percent of the stated elements consists of: from about 40 to 90% carbon, from about 2 to about 10% hydrogen, from 0 to about 40% oxygen, from 0 to about 4 "/ ₀ sulfur, from about 0.1 to about 3% % Nitrogen and from 0 to about 1% chlorine The oil has a calorific value of about 2780 to about 13900 kcal / kg and a specific gravity of about 1 bib about 2. Up to 95 percent by weight of the oil is soluble in water.

The elemental analysis of the waste material, which contains about 70% cellulosic material, The oil hurried here shows that the oil comes from the following Elements by weight percent consists of: from about 52 to about 60% carbon, from about 6 to about 8% hydrogen, from about IVo to un risk 2% nitrogen, from about 29 to about 33 ° o oxygen, and the remainder is made up of small Amounts of sulfur, ash and chlorine are formed. E: It is interesting to note that the elementary Analysis of typical urban waste shows that it is about 46% carbon, about 6% water contains about 6% ash, about 38% oxygen and about 1% nitrogen, where the res formed by small amounts of sulfur and chlorine. This indicates that during pyrolysis nacr the process according to the invention a larger proportion of the oxygen compared to the other elements is lost, probably as CO., unc H..O.

A typical analysis of the oil is given in Table 3 below.

table

Properties of pyrolysis products Properties of animal or bone charcoal

Properties nominal ¹ ) Trial properties Nominal ¹ ) Trial

of the oil area ⁵ ) of the oil area ² )

Calorific value 7.6-lO ^ 7.6 · 10 ^: 'up to calorific value 5000 3333 to 5388

(kcal / liter) 10.6 · 10 ³ (kcal / kg)

Ash content 0.2% 0.20 to 0.6G Ash content 31.8% 21.8 to 50

(Percent by weight) (percent by weight)

Elemental analysis: Elemental analysis:

(Percent by weight) (percent by weight)

Carbon 57.5% 54.5 to 70.6 carbon 48.8% 37.1 to 61.3

Hydrogen 7.6% 6.9 to 9.3 hydrogen 3.9% 2.0 to 4.0

Nitrogen 0.9% 0.6 to 1.5 nitrogen 1.1% 1.0 to 1.5

Oxygen 33.4% 18.9 to 33.4 Oxygen 12.7% 12.2 to 17.2

Sulfur 0.1% 0.10 to 0.20 sulfur 0.28% 0.28 to 0.65

Chlorine 0.3% 0.08 to 0.41 Chlorine 0.22% 0.22 to 0.45

Moisture content 6.3% 4.2 to 10.3 Moisture content 0.6% 0.0 to 1.44

(Percent by weight) (percent by weight)

Flash point 105 ⁰ C ± 10 ° ") -

Density, 21 ° C 1.3 g / cm »-

Solubility test:

Weight percent, soluble in

Water 84%

') On the basis of the currently optimal conditions.

B ^Enzen 47% 2) T _he range depends on the process conditions.

Quinoline 100% η Based on the Cleveland Open Cup technique.

As the table above indicates, the oil produced by the process of the present invention has has a calorific value that is comparable to that of a No. 6 heating oil. The above table also shows 4jass the oil has a density considerably greater than that of water. Thus, the casting of such a öjes do not create the same ecological problems as most petroleum show. If break a tank, for example, in a tanker filled with an oil made according to the invention should or should the oil be accidentally discharged into the sea, the oil would quickly be in the The water will sink and possibly dissolve in the water over time. Although the attempts to As of this writing, there is evidence that the oil is organic Path is degradable.

The invention is explained in more detail below with the aid of a few examples.

example 1

To illustrate the method according to the invention, a sample of urban waste was taken from the city Middletown, Ohio, USA, oven dried at 105 ° C and at atmospheric pressure at 510 ° C pyrolyzed. Preparatory waste recycling was carried out on the sample during the virtually all of the metal, glass, and other materials and approximately 50% of the paper fibers removed became.

The first remaining organic residue of this urban solid waste was continuously fed into a pyrolysis reactor in an amount of approximately 3 pounds per hour and the particle size was between about 0.256 and about 12.7 mm. The results and the chemical composition are summarized in Table 4. the Calorific values are calculated from the respective chemical analysis.

Table 4

Animal charcoal fraction, 36.3 percent by weight;
Calorific value 5400 kcal / kg

61.3 weight percent carbon
2.8 weight percent hydrogen
1.5 weight percent nitrogen
0.4 weight percent sulfur

21.8 weight percent ash

12.2 percent by weight oxygen (difference)

Oil fraction, 28.8 percent by weight;
Calorific value 8200 kcal / kg

70.6 weight percent carbon
9.3 weight percent hydrogen
0.6 weight percent nitrogen
0.2 weight percent sulfur
0.4 weight percent ash

18.9 weight percent oxygen (difference)

Gas fraction, 14.5 percent by weight;
Calorific value 2314 kcal / m ^s

0.1 mole percent water
22.2 mole percent CO
63.2 mole percent CO ₂

2.1 mole percent hydrogen

2.2 mole percent methyl chloride
6.2 mole percent methane

1.8 mole percent ethane

2.2 mole percent C ₁ - to Gj-Konlenwasserstoffe

Water fraction 20.4 percent by weight; contains methanol, acetic acid, etc.

22 "" - '. ^
Example 2

To explain the effect of pyrolysis on the same crushed urban solid waste without prior removal of the paper fibers, but with the metal, glass and inert materials as in Example 1 were removed, the following results were obtained:

Weight percent

Animal charcoal fraction 43.6

Oil fraction 23.7

Gas fraction 13.5

Water fraction 19.2

Example 3

Various urban solid waste with the composition listed in Table 5 below were divided into the three groups identified there.

Table 5

Components in urban solid waste

component

Collected Collected By

by Solid Black Clawson,

Waste Man- Middletown, Ohio,

agement USA
Office

35 Group 1 Weight
percent,
dry
Base Weight percent,
dry base Metals 40 Glass 11th dirt 10 Group total 3 45 Group 2 24 27 Food waste plastic 17th Garden waste 5 5 ° Fabrics 4th wood 3 Group total 2 55 Group 3 31 20th paper total 45 53 6o mn -inn

Groups 2 and 3 of the Blaclc Clawson Company waste classification were combined and torn to 0.5 mm, resulting in a waste feed yield of the approximately 90% inorganic Fabrics were removed. This waste charge was reduced to less than 5% in the oven

Moisture dried and pyrolyzed at about 500 ° C and atmospheric pressure without hydrogenation, in the manner described in Example 1, which resulted in a yield of products such as they are summarized in Table 2 given above.

Example 4

The oil fraction from Example 3 was subjected to atmospheric distillation resulting in nine cuts which are given in Table 6 below.

Table 6

Atmospheric distillation of oils from the
Pyrolysis of solid waste

section

Distillation temperature
Area

Product in
Weight percent

1 104 to 132

2 132 to 160

3 160 to 188

4 188 to 216

5 216 to 243

6 243 to 271

7 271 to 299

8 299 to 327

9 327 to 346
rest

Loss + in the apparatus
remained

10.3
9.9
7.0

12.1
3.5
2.3
1.3
1.4
0.7

32.4

19.1

dwell time of about 1.1 seconds in the pyrolysis zone. The liquid organic chemicals and fuels d. H. the oil produced had a moisture content of 20 percent by weight. The solubility of the oil was examined with regard to several solvents and solutions, the results of which this Investigations are summarized in the following Table 7.

Table 7

Produced oil at 20% moisture content

solvent

Solubility of the oil
(Weight percent)

20 Aqueous alkaline soda 99.5 Methanol 95 acetone 95 ₂₅ quinoline 98 Water pH 4
pH 6
pH 2 63
59
67 ³⁰ ammonia pH 10 70 benzene 8th toluene 8th 35 hexane 2 Glycerin
40 15 to 40% depending on
of the absence
term of organic chemi
with caustic and fuel
high molecular weight

The oils tested were formed by the residue of a vacuum distillation in which acetone was stripped off, the final solution temperature being approximately 52 ° C. The mass balance for the oil-producing run was 80%, and the remaining 20% non-recovered material is assumed to be ¹ A has been reached because of the distillation losses. It is estimated that 9 to 13 Vo of the weight of the oil produced was lost due to the low boiling point fraction boiling below 104 ° C.

Example 5

Sorted and shredded municipal waste (more than 75% of cellulose-like material, less than 10 ⁰ Zo inorganic substances) of pyrolysis was subjected in the manner described in öeispiel 1 manner, a turbulent gaseous stream was used consisting of 16 _^2/3 percent by weight of carrier gas 1673 % particulate! Municipal waste and 66V3 weight percent particulate animal or bone charcoal. The particulate solid waste was heated to a temperature of approximately 510 ° C and had a consistency

Example 6

Crushed rubber tire stock (69% carbon, 7% hydrogen, 0.3% nitrogen, 1.1% sulfur, 17.5% oxygen, and 4.4% ash) was pyrolyzed in the manner described in Example 1 to approximately 33% particulate Animal or bone charcoal to make about 17% gases (chemicals and fuels) and about 50% liquid chemicals and fuels. The elemental analysis of the liquid showed the following substances: carbon 83%, hydrogen O 9 ^0, 0.7% nitrogen, 1.1% sulfur, oxygen, 4.0% ash and less than 1.0%. The specific gravity of the liquid was approximately 1 and the oil had a calorific value of approximately 10,000 kcal'kg.

Example 7

Douglas spruce tree bark was crushed to a sieve fineness of 0.5 mm and as described in Example 1 pyrolyzed. The produce was 18% coal, 48% oil, 20% gas, and 8% moisture.

609 634/186

/ OO

The elemental analysis of the products gave the following values:

Animal or oil

Charcoal gas

carbon

hydrogen

nitrogen

sulfur

ash

chlorine

oxygen

Carbon monoxide

Carbon dioxide

methane

C, H "and C ₂ H ₄

C ₃ to ^ hydrocarbons

The products had the following calorific values:

Coal 6400 kcal / kg

Oil 6700 kcal / kg

Gas 4450 kcal / m ³

66.0 60.7 - 4.1 8.0 9.1 percent by volume 0.2 0.2 - 0.0 0.0 - 7.5 0.05 - 0.03 0.01 --- 22.0 31.0 - - - 47.1 percent by volume - 21.4 percent by volume
11 fi 0 '" - - L1 , U / 0
5.8 percent by volume

5.0%

Example 8

Rice husks (37.7% carbon, 5.3% hydrogen, 0.4% nitrogen, 0.02% sulfur, 0.18% chlorine, 18.8% ash, of which 78.9% am, SiO ₂ , 33 , 5% of oxygen and 4.1% of H ₂ O) were comminuted to 0.5 mm sieve fineness and pyrolyzed at 500 ° C in the manner described in Example 1 to give a yield of the following products: Oil 31 %, Animal or bone charcoal 56% and gas 13%. The coal consisted of 63.4% carbon, 2.0% hydrogen, 2.0% nitrogen, 0.5% sulfur, 0.11% chlorine, 27.4% ash (about 75% of which was SiO ₂ ) and 4.6% oxygen.

Example 9

Tetracosane was ground to a sieve fineness of 0.13 mm and pyrolyzed according to the invention. The tetracosane was combined with a turbulent gaseous stream which was essentially free of oxygen and was inert to the tetracosane. Hot particulate animal or bone charcoal at 980 ° C was added to the turbulent gaseous stream (5 pounds of coal per 1 pound of tetracosane) and the entire mixture is passed into the pyrolysis zone for a residence time between 1 and 5 seconds in order to obtain the Tetracosane to a temperature of about 815 ° C heat to thereby form liquid chemicals and coal from fuels. These substances were quickly called after leaving the pyrolysis zone, cooled to a temperature oil door below 260 ° C. The elemental analysis of oil of the liquid chemicals and fuels obtained in this way was as follows: approximately 85% Carbon, about 15% hydrogen and about 0% oxygen.

ExampleO

The procedure of Example 9 was repeated using 2 pounds of animal or bone charcoal per 5 LJm ς i ^5tr * ^{cosane and a} residence time between Jv Y} ^{onds to} give a liquid chemical and fuel similar to that used in Example 9 was recovered.

Example 11

to about 94% V? * ^ y
Hydrogen ,, ^ ¹ U ^K ° ^hlenstoff. about 6% hydrogen and about 0% oxygen.

Example 12

^Bcis P ^5el ^ 1 ™ rde repeated, T ^{Na Phthalin} to carrier gas? ^{6 dwell times} from less ^ve ™ ends to a

^{that obtained in} Example 11

Example 13

< ^{30 /} "humidity) ^{Sieve fine} <* -rklei-

Number 3000).

The weight ratio of particulate! Manure to gas to coal is 1: 1: 4. The turbulent gaseous Stream was passed through a pyrolysis zone with a residence time of approximately 0.8 seconds, in order to form organic liquid substances, which quickly after leaving the pyrolysis zone to a temperature were cooled below 235 ° C.

Example 14

Municipal rubbish dried in the oven (1%> humidity), that contained less than 5% metal, glass or other inorganics was reduced to less than 3.175 mm sieve fineness crushed and flushed with nitrogen to remove the oxygen it contains. The waste, which contained less than 1%> oxygen, was placed in a pyrolysis reactor under a nitrogen atmosphere entered to prevent the entry of air, and combined with a carrier gas, which was essentially free of oxygen and inert to the garbage, and continued to be hotter

Animal or bone charcoal (temperature = 735 ° C) to form a turbulent gaseous stream (Reynolds number 2000+). The stream had a rubbish to gas to coal ratio of 1: 2: 2. The turbulent gaseous flow was caused by a (Reynolds number 2000+). The stream was directed at a temperature between 425 and about 510 ⁰ C to form organic chemicals and fuels. After leaving the pyrolysis zone, these substances were rapidly cooled to a temperature below 150 ° C. in a cooling tower and taken up in a phase separation tank.

Example 15

The procedure of Example 13 was repeated using a ratio of crushed manure to gas to charcoal of 1: 1: 10 was used and the charcoal heated to a temperature of 1550 ° C was used to heat the manure in the pyrolysis zone to a temperature of approximately 1400 ° C.

1 sheet of drawings

Claims (13)

Patent claims: I. A process for the production and recovery of chemicals and fuels from waste containing organic solids, in particular waste, characterized in that a particulate waste material containing less than 10 * Ό inorganic substances and hot particulate animal or bone charcoal with a carrier gas which is inert with respect to the waste material form a gaseous stream is combined and the gaseous stream with turbulent flow is passed into a pyrolysis zone for a dwell time of between 0.05 to 10 seconds, in this case the waste material is heated ^{to a temperature in the range between 150 and 1400: C with the formation of organic chemicals and fuels} and that the organic chemicals and fuels are removed from the pyrolysis zone or that the particulate animal or bone coal and the organic chemicals and fuels are removed together from the pyrolysis zone and that the animal or bone coal is then removed is separated from the chemicals and fuels and, if necessary, a part of the solids removed from the pyrolysis zone is heated and returned to the circuit for the formation of the turbulent gaseous flow. 2. The method according to claim 1, characterized in that that the organic chemicals and fuels discharged from the pyrolysis zone a temperature below the p> rolysis temperature can be rapidly cooled. 3. The method according spoke I or 2, characterized in that the residence time of the waste material is maintained in the pyrolysis zone at less than about 1 second. 4. The method according to any one of claims 1 to 3, characterized in that the waste material is heated in the pyrolysis zone to a temperature between 315 and 565 ° C. 5. The method according to any one of claims 1 to 4, characterized in that before heating in the pyrolysis zone essentially contains the inorganic substances contained in the waste material be completely separated. 6. The method according to any one of claims 1 to 5, characterized in that the particle size of the waste material is brought to a maximum dimension of less than 2.5 cm. 7. The method according to any one of claims 1 to 6, characterized in that the separated, in Animal or bone charcoal returned to the cycle to a temperature between 620 beforehand and heated to 980 C. 8. The method according to any one of claims 1 to 7, characterized in that an amount of carrier gas with the particulate waste material and the hot, particulate animal or bone charcoal is combined which is sufficient to produce one to form a turbulent gas storm with a Reynolds number of at least 2000. 9. The method according to any one of claims I to 8, characterized in that the weight ratio from carrier gas to particulate! Waste material between 0.2: 1 and about 2: 1 in the turbulent gaseous flow is set. IU. Method according to claim 9, characterized in that that via controlling the amount of particulate animal or bone charcoal that particulate waste material in the pyrolysis zone to a temperature between 150 and 815 C is heated. 11. The method according to claim 10, characterized in that that the weight ratio of hot, particulate animal or bone charcoal to particulate! Waste material in the turbulent Gas flow is adjusted to at least 2: 1. 12. The method according to any one of claims 1 to H, characterized in that the carrier gas a hydrogen enriched gas stream is used. 13. The method according to any one of claims 1 to 12, characterized in that the waste material is solid waste, in particular municipal waste, Manure, sewage sludge, automobile tires, untreated process waste, agricultural waste, industrial waste, Tree bark, rice husks or mixtures of these substances is used. b *. Method according to one of claims 1 to 13, characterized in that the waste material has a moisture content of less than 5 percent by weight is brought. 15 Liquid organic compound and fuel obtained from a waste material containing organic solids by combining the particulate waste material, which contains less than 10 ° o inorganics, with hot particulate animal or bone char and a carrier gas which, with respect to the waste material, is contained in the is essentially non-oxidizing to form a turbulent gaseous stream, the turbulent gaseous stream was passed into a pyrolysis zone for a residence time between 0.05 and about 10 seconds, in which the waste material with the formation of liquefiable organic chemical compounds and fuels by appropriate choice of Temperature of the particulate animal or bone char in the pyrolysis zone to a temperature between 150 and 1400 ^; C was heated and the chemical compounds and fuels were condensed.