CS222655B2 - Method of making the fuel from cellulose materials - Google Patents

Abstract

Cellulosic material, is converted into a useful, low-sulfur and low-ash coke type fuel by autoclaving at a temperature of 750 to 1250 DEG F and pressure of at least 1000 psi for a period of time to convert the moisture and a portion of the organic constituents therein to a gaseous phase and to effect a controlled thermal restructuring of the chemical structure of the cellulosic material, producing a solid coke-like product and a by-product fuel gas. The low- sulfur coke product can be comminuted and admixed with high- sulfur fuel oils, providing a blended liquid slurry fuel of acceptably low- sulfur content. <IMAGE>

Description

BACKGROUND OF THE INVENTION The present invention relates to a process for producing fuel from cellulosic materials, in particular waste, for a valuable fuel with poor sulfur content and low fuel content. Well, I'm going to seed the ashes.

There is a method of improving the quality of lignia type coal including lignite, lignite and pitch brown UJ to be ui. due to thermal change in chemical structure, it is more suitable as a solid fuel. The resulting higher quality carbonaceous product is stable, weather resistant and has an increased calorific value approaching black people. In this way, lignitic carbon from large domestic deposits can be converted to useful fuel, which is one possible solution to the energy crisis.

In addition to large domestic deposits of the Ligni type, large amounts of cellulosic type are produced each year, which are both naturally occurring, such as peat, and waste from logging and agricultural work; these materials are in a form that is not suitable for use as a commercial fuel. Waste cellulosic materials such as sawdust, bark, wood waste, branches and splinters from logging, and various agricultural waste materials, such as the stalks of a Bavarian, will present a major problem from KLEAL HOLDING. Therefore, there has been a long-term search for ways to convert such cellulosic maize to a valuable fuel, thereby not only partially solving the fuel shortage problem, but also eliminating or at least altering the cost of disposing of these waste materials.

In addition to these problems, there is another serious environmental problem where national standards allowed the sulfur content of fuel oils that can be combusted in electricity and steam generating plants to about 0.7% of the total, while in some countries maximum permits are allowed. sulfur content only 0.3%. lmoUnitnícl ·. In order to comply with these regulations, it has hitherto been necessary to mix fuel oils of domestic origin having a relatively high sulfur content with low-sulfur fuel oils imported from heaters to form a sulfur-containing mixture within the permissible limits. The import price of low-sulfur fuel oils makes the process not only expensive but also increasing the dependency of foreign sources.

SUMMARY OF THE INVENTION The present invention provides a method for producing fuel from cellulosic. materials that eliminates the problems mentioned. According to the invention, the batch is heated in a xutuclav ox at a temperature of 400 to 677 ° C at a pressure of 7 to 23 MPa, the water and the volatile organic components are converted into a gaseous phase with simultaneous thermal transformation of the chemical structure and chemical composition of the batch. The sugar product is cooled and optionally ground. Gaseous phase during processing in the reactor, it is discharged from the reactor and allowed to condense before cooling, the non-condensing components being treated as a gaseous fuel.

According to a further preferred embodiment of the invention, the cocoa product is ground to a particle size of less than 48 mesh, preferably less than 200 mesh, and suspended in fuel oil at 1 to 50% by weight of coke, calculated on total blend forming a liquid heating slurry. For example, peat, agricultural wastes, wood wastes and their waste are used for the production of coke products.

The invention makes it possible to treat waste celluloses of the type which have been orphaned and have generally been disposed of into a valuable high calorific coke fuel having a low sulfur and ash content. The ground coke can be added to high sulfur fuel oils and its properties make it possible to form stable suspensions without the need to add suspending suspension chemicals; the low sulfur content of the coke, lying around 0.1% by weight, and the ash flying from 1 to 4% by weight, ensures that the fuel mixture complies with all requirements and in particular the regulations regarding the sulfur content.

The invention will be explained in the following description in conjunction with the drawing x exemplary embodiments. While the drawing shows the sequence of the individual working processes of ktrrých trttáiá ^of the inventive method.

The cellulosic feedstock or a mixture of different cellulosic materials is fed from the container J to a pre-treatment stage 2, where the feedstock is crushed, milled and sieved to produce a feedstock of appropriate particle size; the ground material is then fed to a high temperature high pressure reactor 3, where it is subjected to heat and pressure, to extract moisture and volatile organic compounds and to convert the thermal decomposition products into gases, without the thermal transformation of the chemical structure of the carbonaceous feed.

The gaseous by-products are removed from the reactor 3 and fed to the condenser J from which the condensable phase is taken as condensate, while the non-condensable phase is taken as a by-product gas which can advantageously be recycled and used directly in the method of the invention and for generating additional energy. The reaction products flow from the reaction zone of the reactor 3 to the cooling zone g, in which they are cooled to a temperature at which they can be exposed to occlusal atmospheres without incineration or other adverse events. From the cooling zone 2, the solid reaction product or the coke formed is transferred to the coke tank 6.

According to a preferred embodiment of the invention, the resulting coke is passed from the container 6 to the crusher J where it is further crushed to a powder of the desired grain size, making it suitable for use as a pulverized solid fuel according to the special type of furnace and burner to be used.

For this purpose, it is fed into a storage vessel 8. According to the invention, part of the pulverized powder coke can also be introduced from the crusher. 1 into a mixer 2, where it is mixed with fuel oil supplied from the oil tank 10. This produces a slurry which contains a controlled amount of suspended ground coke. The resulting prodlet consisting of the fuel oil and the ground coke is passed from the blender 2 to the storage tank 11 for the mixture of fuel oil and powdered coke.

In the process of the present invention, the batch material may contain a wide variety of cellulosic materials or a mixture of cellulosic materials, including cellulosic wastes arising from the logging and processing of wood and agricultural waste. For example, natural cellulosic materials such as peat and waste cellulosic materials, such as sawdust, bark, wood residues, branches and chips, can be used, as well as various agricultural waste materials, such as cotton stems, nut shells. , shelled corn cobs - and similar waste.

Pretreatment of the batch material prior to introduction into the reactor 3 This may include a treatment to remove excess water and thus reduce residual moisture to a value that facilitates further processing and manipulation and reduces the moisture content of the next reaction in reactor J.

Since substantially all of the moisture from the charge is removed during heating in an autoclave, this pre-dewatering is not necessary for most agricultural and wood waste. The pretreatment involves crushing or grinding the batch, thereby converting the batch particles in the flask, by its nature, to a dimension facilitating manipulation and processing. The crushing and milling may be followed by screening or sieving to remove excessively large particles which are fed back into the crusher.

The pretreated or optionally untreated charge material is then introduced into the inlet port of the reactor 3 in which it is subjected to a temperature of at least 400 ° C and a pressure of at least 7 MPa for a predetermined controlled time interval to effect controlled thermal transformation of the chemical structure and moisture conversion. and volatile organic compounds as well as gas-phase thermal decomposition products. This gaseous phase is withdrawn from the reactor and is preferably fed to a condenser 4 in order to read off the condensable phase containing the valuable byproduct chemical compounds.

The non-condensed gas phase condensation withdrawn from the condenser 4 can advantageously be used as a gaseous fuel to heat the reactor 3 and to generate auxiliary energy for the entire process, while the excess energy remains available for sale.

Although temperatures of at least 400 ° C are desirable in the autoclave treatment, a temperature of about 540 ° C is most advantageous since it rapidly evaporates and thermally converts the batch structure to produce a high solids content product. This reduces the residence time in the autoclave and increases the efficiency of the process. The processing temperature in the autoclave may be. up to 700 ° C, and temperatures above this value are usually undesirable because too much condensation-free gases are produced relative to the solid coke product. Particularly satisfactory results were obtained at temperatures ranging from 540 to 650 ° C at a pressure ranging from 7 to 21 MPa. The maximum applicable pressure is about 23 MPa. Higher pressures are undesirable, especially because of the high cost of manufacturing tic containers capable of withstanding these high pressures, and because at pressures above 21 MPa, neither improvement nor acceleration of the process occurs.

The residence time of the carbohydrate in the automobile varies depending on the ratio of temperature, pressure and time, which is controlled to such an extent that substantially complete moisture is present and some of the vapor evaporates. volatile organic compounds and for the controlled thermal transformation of the ce-charge structure.

The nature of the thermal transformation of the structure is not entirely clear, but is believed to be based on two or more simultaneous chemical reactions between the pyrolysis products and the gases that are present in the cell structure of the cellulosic feedstock. These structural copper reactions result in changes in chemical properties that result in an increase in the carbon to hydrogen ratio and a reduction in the sulfur and oxygen content, which can be measured by analysis of the produced coke.

During the treatment in the flow, a controlled thermal transformation of the structure and / or decomposition of the chemical structure occurs, accompanied by the formation of additional gaseous components, which also pass into the gas phase.

The required residence time in reactor J 'decreases with increasing temperature and pressure. Conversely, in the event of difficulties in lower temperatures and pressures, a longer residence time in the aluminum is required. Typically, a residence time in the range of about 15 minutes to about one hour at temperatures ranging from 485 to 650 ° C and pressures between 7 and 21 MPa is satisfactory. Results have also been obtained for some materials at temperatures and pressures at the upper limit of the allowable size, with a dwell time of only five minutes, while a dwell time of more than one hour is also a cell. In general, a dwell time of over one hour does not yield significantly improved results over a defined range of 15 minutes to 1. The reduced throughput and the lower efficiency of the process associated with such a long residence time is undesirable from an economic point of view.

The pressure increase over the autoclave can be advantageously effected by controlling the cellulosic feedstock with respect to the internal volume of the autoclave, taking into account the content of the feedstock, so that, when the feedstock is heated to an elevated temperature, such a gas phase consisting of superheated steam and volatile organic components to increase the pressure in the OH to the desired pressure range. If necessary, the pressure in the autoclave can be additionally increased by introducing pressurized gas or pressure gas or pressurized steam.

After processing. In either preferred embodiment of the invention, the autoclave can be left to autoclave, for example by air cooling or a coolant, for example water, to a temperature at which the solid coke can be exposed to air without harmful effects. Zpravila is PhLi ^ z ^ OCM-eddi autoclaving at toploto ^ ^p o ^d 1 ⁵ ° C. This at or near 100 ° C is undesirable in the gas phase, since the aqueous gas phase condenses and the male coke produced, thereby increasing its moisture content and thereby reducing the calorific value. Preferably, the cooling is carried out after the gas phase has been removed so as to prevent condensation of the vaporized organic components, including the relatively hydrocarbon fractions and tars, and thus their deposition on the surface and in the coke pores.

The produced coke of improved quality usually has a matt black, porous appearance. structure and residual. moisture content ranging from 1 to 5% by weight.

According to a preferred embodiment of the invention, after the autoclave treatment, the remaining high pressure inside the autoclave is released at the working temperature and the hydrocarbon components are recovered by condensation, while the non-condensable organic gaseous components are removed as fuel by-product. Under these okoonooties there is only a slight deposition of the evaporated organic components on the produced coke. The coke produced in this way is, however, characterized in that it has a thermally converted structure which has an increased calorific value.

According to the invention, a two-stage autoclave treatment and coating process can also be carried out in which the gas phase released from the autoclave at operating temperature is transferred to a second autoclave chamber where the feedstock to be treated is used as a cooling medium to condense tar and oil from gas phase.

The cooled solid produced coke is transported from the cooling zone - as shown in the diagram - to a coke tank from which it can be transported in containers or freely; 1 ^ ^ 0X01111101 coke can further _{zprccovával>} in an appropriate grinding or milling to break up agglomerates formed during the treatment in the autoclave and to prodlet milled to the desired average particle size. The degree of comminution of the produced coke depends on its intended use and on the specific design of the burner that will be used to burn the coke as a pulverized solid fuel. For example, when the produced coke is to be used in burners of a type suitable for burning pulverized coal and similar fuels, useful particle sizes are less than about 48 mesh and preferably less than about 200 mesh. Alternatively, the produced coke may be used in automatic stoking ovens where its particles may be larger in size.

Regardless of the particle size, the coke produced is a valuable solid fuel and can be used directly in this shape or in general with other conventional fuels. The coke produced is characterized by a very low sulfur content, usually less than about 1% by weight, mostly from 0.2 to about 0.06% by weight. In addition, the produced coke is characterized by a very low ash content, usually less than 5% by weight and possibly less than 1% by weight. Some agricultural waste materials, such as cotton stalks, coke with an ash content of about 20% by weight and a sulfur content of less than 1% by weight. Typically, the coke produced has a calorific value in the range of 25,580 to 34,890 kJ / kg.

Due to the very low sulfur and ash content of the produced coke, the coke can advantageously be used in a fuel mixture having a high sulfur content, resulting in a resulting fuel mixture having a substantially lower average sulfur content and thus corresponding to national and local requirements prescribing sulfur content.

Although the milled coke according to the invention can be advantageously mixed with pulverized solid fuels, for example with various kinds of hard coal and coke, particularly advantageous results are obtained when the coke is mixed with fuel oils in a liquid slurry containing from 1 to 50% . The maximum coke content contained. in this heating slurry, it is bypassed to increase the slurry viscosity while increasing the ground coke concentration. The coke concentration in the chest is such that the slurry has a suitable aisliste so that it can be pumped, at which viscosity results in an adequate atomization at various conventional burners. Although slurry concentrations of only 1% hmmt are contemplated. at such low concen- tration, essentially the advantage of the invention is achieved by mixing the oils with a low-sulfur-containing coke. pojpBla; as a result, concentrations of at least 25 to 50% by weight are preferred. At a concentration of about 50% carbon, the average sulfur content of the slurry is about half that of the high sulfur oil, making it possible to utilize the more refined high sulfur fuel oils to produce accepted heating grades conforming to national and local standards.

It has been found that the addition of ground coke having a particle size of about 150 meah with an initial distribution where 80% of the particles are smaller than 200 mesh produces a relatively stable slurry at 50% by weight of coke and 50% by weight of fuel oil. to use larger amounts of additional susceptible agents to provide stability. Usually, it is not necessary to use agents to maintain the compositions, whereas in the case of conventional hard coal and anthracite with oil such agents are necessary. As a result, a substantially simpler composition is achieved. and reducing the cost of the resulting mixture.

The following examples illustrate the process according to the invention and do not in any way limit the scope of the invention.

Example 1

A cellulose charge containing 59.5 g of a mixture of dry oak and fir wood is placed in a test reactor together with 23.4 g of water. The wooden charge is in rods whose base rnměí 6.35. 12.7 mm and length 203.2 mm.

The test reactor consists of a cylindrical stainless steel chamber having an inner diameter of 34.925 mm and a length of 305 mm, so that its total volume is 295 cm ³ . The reactor is provided with a conduit connected to a water-cooled condenser and a gas collector. A pressure gauge with a scale of 35 MPa is connected to the reactor for simple pressure control, and the K-type thermoelectric cell is housed in the reactor well for full temperature control. The system includes a conical high pressure veenil in the conduit between the reactor and the gas condenser to discharge the gas phase from the reactor and maintain the necessary pressure in the reactor chamber.

After filling and closing. The reactor is placed horizontally in a heated morphine furnace. After 5 min. the reactor pressure rises to 10.5 MPa and the internal temperature indicated by the tero-electrocircuit to 295 ° C. At this point, the discharge valve opens slightly and a mass of gas is discharged through the condenser to maintain a substantially constant pressure of 10.5 MPa in the reactor. During the following 5 minutes, or for a total of 1010 minutes after the reactor was placed in the melt furnace, the temperature inside the reactor indicated by the thermocouple increases to 544 ° C. The reactor is ^P and the ^y JME from - the furnace and the necW och ^ dl-t about ⁹³ ° C.

After opening, the solid produced coke of 18.9 g and 20 cm 3 of fluid was removed from the reactor. Mioožsví resulting gas is greater than the collecting kaFeac ^ to ^ b ^ ^kt era has about 7800 .mu.m ш ^third

Visual inspection of the solid coke product produced shows that the coke has a black color and a honeycomb structure which substantially corresponds to the flood structure of the cellulosic wood charge and has the appearance of a coke fluid in many places. The original oak and fir wood monoelectric rods are deformed during the reaction so that the solid product obtained has the shape of a single cylinder with a smaller diameter than the diameter of the reactor chamber.

The gaseous phase obtained burns with a light blue flame, which is typical of hydrogen, carbon monoxide and (^ βηο ^). The solid product has the following composition:

humidity (% 1шо ^) 3,93 volatile components (% hmo ^)

8.82 ash (% 1шо ^)

1,13 bonded carbon (% Iocoi)

90.1 net calorific value (kJ / kg) 33 287

653

Chemical composition:!

C (% hiOO)

88.8

92.4

2.06

2.14

0.12

0.12

0.18

0.19

3.82

4.02

Example 2

Charge of Canadian peat from raáeliník hmoOnooSi 100 g load! to the test reactor described in connection with Example 1 and provided with condensers, one of which is steam-cooled and the other water-cooled. Analyzes of charge · mattritl show that the moisture content is about 75% of the mono-monosity.

After filling, the reactor was placed in a horizontal position in a heated soap furnace as described for Example 1. After 11 min, the pressure in the reactor was increased to 11.5 ° C and the internal temperature indicated by the terioelectric coupling to 264 ° C. In this process, the gas discharge valve was slightly opened and the gas was released from the reactor through a condensation system so that the pressure inside the reactor was 10.5 MPa.

After an additional heating time of 23 minutes, or a total of 34 minutes after the reactor had been placed in the quench furnace, the temperature inside the reactor was 544 ° C. The reactor is then removed from the furnace and the high-pressure discharge vent is opened to discharge all the gas phase and the reactor chamber is pressurized. The verntl is then sealed and the reactor is allowed to return to ambient temperature.

At the end of the experiment, the steam-heated condenser contains 74 g of liquid, while the water-cooled condenser contains 5 g of liquid 4,2 4.25 L of non-condensable gas is trapped in the gas collector. The reaction product has a homogeneity of 6.99 g and a visual control shows that it consists of a brittle, black solid product which gives 0.256 g of ash upon oxidation.

The gas which, when ignited by Blue Flame, has the following composition:

Folder mo. percent hydrogen water oxygen hydrogen sulfide argon carbon dioxide methane ethane ethylene propane ppylene isobutane n-butane

4.96

0.24

Ц23

0.00

0.11

52.51

19.24

2.13

0.12

0.29

0.14

0.02

0.05 continued

Component Indian. percent butene 0.03 izopeotan. 0.01 o-pentao 0.01 pentene 0.02 hexane 0.00 heptane 0.05 beozeo 0.38 octane 0.00 toluene 0.09 oooao. 0.00 sylen 0.00 nitrogen 14.44 carbon monoxide 3.93 Calorific value (kJ / m ^) 11 370

Example 3

The test described in Example 2 was repeated using 173 g of the same peat charge and the same apparatus. 8 min after insertion of the reactor into a mule furnace, the pressure inside the reactor was 10.5 MPa and the temperature in the reactor chamber was 232 ° C. After a further 21 minutes at the same temperature, or a total of half29 minutes after the start of the heating cycle, the temperature in the reactor is 540 ° C and the pressure is maintained at 10.5 MPa by discharging the gas phase into the condensation

In the steam-heated tandenzátoru the CIS and the total volume ^{to 58} cm deep ^{P h} while oědé tetatio ^ c ^h a water bath ^for about ^h ondenoátoru the ZTO ^ ⁶ Cu 3 ^P yellow water. The ^{p s} Lynn collecting system is collected by the total m ^ n ^ s ^^ ožst 11.2 1 gas. A solid produced coke of 19.2 g, similar to the product of Example 2, is obtained from the reactor. After ignition, the gas burns with a blue flame as in Example 2.

The solid coke produced contains 0.41% moisture and mine in the dry matter and elemental composition according to the following table:

Quantum Analysis% УmoOnootic Peat charge Made solid coke volatile components . 77.5 6.34 ash 1,22 4.4 bound carbon 21.3 89.3 higher calorific value (kJ / kg) 20 '241 33 620 Features (St hr.) C 51.8 90.7 H 3.14 3.35 WITH 0.15 0.14 N 0.61 0.83 0 43.0 0.61

The solid coke produced on the basis of dry matter clearly proves the increased calorific value of the coke !! 66%, and it is a very royal solid fuel with low ash and sulfur content. Following grinding to about 200 mesh particles, the product is ideally suited for mixing with residual fuel oils of high sulfur content to form a slurry fuel for burners having a low sulfur content.

The oil slurry is prepared by mixing the finely ground coke produced from the peat according to the process of the invention in the same mole ratio with the residual fuel oil containing 1% mmoono-sulfur. Suspension of the coke particles in the fuel oil is achieved by adding powdered coke to the fuel oil while stirring in a high speed plate. The produced coke is added in such a quantity that its concentration is about 40% of the hooonoot total slurry hmoonoosi.

The resulting fuel oil slurry has an average sulfur content of 0.66% hmoonoot, making it suitable as a fuel in power plants and conforming to all national and local standards for the maximum sulfur content. The slurry produced by mixing residual fuel oil and powdered coke is substantially stable, and the coke particles are uniformly suspended without the need for suspending and / or dispersing agents.

Example 4

Typical batch vbsthující wood residues, bark and · of firs and pines in the oooossví 51.76 g vvooí poppaného into the reactor in the first ppřkladu After 7 days шОп dosátane pressure 11.5 1mA and ^p ly ^ ⁿ b ^y vypcou pressure ZAsILaX kvnstanOní. The reactor temperature is 283 ° C. for a further 13 min, the temperature in the reactor was raised to 532 ° C, keeping the pressure constant at 10.5 MPa by discharging the gaseous phase to the condensation system. 17.9 g of solid coke product and 15.8 g of liquid are obtained.

The product from the steam condenser consists of 5.3 ml of yellow liquid to which pLave 0.6 ml of tar material. The water condenser product consists of 10.5 milliliters of clear liquid with traces of oil. Tetanina from both condensers were mixed and then 14.6 ml of water, 0.254 grams of soluble tars in hexane and 0.28 g of soluble tars vb ^e nz ^en u. Simultaneously with ^e zííská about ⁹⁰⁰⁰ cm @ ³ of yne nescho ^^ condensation. The composition and calorific value of the solid coke produced and the gas phase composition of the non-condensable gas are given in the following table:

Solid product composition and calorific value

Solid product (kg / kg of charge) 0.346% moisture percentage 0.27% first analysis, (dry matter) volatile carbon-bound ash

11.04 84.09

4.87 elemental analysis (dry matter)

C

H

WITH

N

88.58

2.71

0.06

1.36

2.42

Calorific value (kJ / kg)

313

Composition of produced gas

Volume of produced gas (ltry / kg charge) average mol. mass, calorific value (kJ / m ^)

Composition of mole percent (dry matter) H ₂

CH ₄ co c ₂ co ₂ ^c 6

180,4%

31.9

979

5.87%

29,32%

7.55%

4.65%

50,19%

0,99%

0.4.7%

0.26%

0,40%

Example 5

The reactor experiment described in connection with Example 2 was repeated, but using 51.8 g of cellulosic feed material containing agricultural waste consisting of cotton stems and capsules. The reactor pressure reached 10.5 MPa 6 minutes after placing in the muffle furnace, the internal temperature of the reactor being 217 ° C. At this point, the discharge valve is opened and the gas phase is discharged to maintain a constant reactor pressure of about 10.5 MPa. After a further 17 minutes of heating in the muffle furnace, the temperature is 541 ° C, after a total reaction time of 23 minutes, and the gas is continuously discharged to maintain a constant pressure.

10.5 MPa. At the end of this time, the reactor was removed from the furnace and the pressure reduced to atmospheric. The total amount of gas produced was 11,240 cm @ 3, the total amount of solid product was 16.1 g, and the total amount of tar was 0.6 g.

The composition and calorific value of the solid coke produced and the gas phase composition of the non-condensable gas are shown in the following table.

Solid product composition and calorific value

Solid product (kg / kg charge) 0.310 percent moisture8 1,58% first analysis (dry matter) volatile components 17.45 « bound carbon 62,00 ash 20.55 «

Elemental analysis (dry matter) C 72.28 % H 2.62 % WITH 0.69 % N 1.20 % 0 2.66 % Calorific value (kJ / kg) 26 792

Composition of produced gas Volume of produced gas (liters / kg of charge) 217,00 average moo. 29.2 Calorific value ⁽ Ы / п ³⁾ 20 151 Composition of mol percent (without humidity) h ₂ 10.30 % 0H ₄ 34.44 % what 3.66 % ^C 2 4.01 % co ₂ 44.97 ^C 3 1, 40 % ^C 4 ’0.87 % ^C 5 0.18 % ^C 6 0.17 %

Example 6

To test the reactor was loaded batch consisting of 60 g of wood shavings from ¹ 5 ³ CN · Water test system of the reactor sesrárá cylindrical chamber of nerezaaějící OCE ^L to a diameter of 31.75 nm and ^d ELCÉ 336.21 cm, that is the volume of ^{the O} , 461 5 m ³ . The reactor is provided with a conduit leading to a water-cooled condenser and a gas collector. A pressure gauge of up to 35 MPa is connected to the reactor for continuous pressure control, and a K-type thermocouple is housed in the reactor well for a convenient temperature control. The assembly includes a conical high pressure valve located in the conduit between the reactor and the gas condenser to discharge the gas phase from the reactor and maintain the necessary pressure.

After filling and closing, the reactor is placed horizontally in a heated morphine furnace. After 9 min, the pressure inside the reactor is 12.3 MPa and the temperature indicated by the thermocouple is 249 ° C. At this point, the outside of the reactor is slightly opened and a gas stream is discharged through the condensation system to maintain the pressure inside the reactor at a constant value of about 10.5 MPa during a subsequent period of 21 minutes, or for a total of 30 minutes. placing the reactor in a high-speed furnace is a reactor temperature of 540 ° C; then the reactor is removed from the furnace, pressure. The reactor is allowed to cool in air.

Detects ^gp evného ^{14.6 to} about ^the SU ^{11200 cm-3} to ého pl ^y nu incompetent ^to enzace en ^d, so that the solid consists of 24% hmžentetních. The solid coke product produced is coke-like in appearance and has a brittle porous structure. Condensation incapable of combustion gas burns with a yellow end.

The produced solid product is ground in a laboratory ball mill for 10 min and then sieved through a 200 mesh sieve. The remainder of the fraction greater than 200 mesh was ground for 10 minutes and sieved again. The fractions above 200 mesh are ground for a further 5 minutes, after which time 12.75 g is passed through a 100 mesh screen and 8.69 g through a 200 mesh screen. 12.75 g of milled solids are added to 8.52 g of fuel oil to form a solid paste containing 60% by weight of solids. Additional oil is added to this solid paste until all cavities are filled. At this stage, the paste has 56% of phenolate solids. Additional oil is then added until the mixture flows at room temperature. This mixture contains 52 Ά weight of solids.

A second batch of oil and solids slurry was prepared from a similar manufactured coke prepared from wood, which was ground in a ball mill and passed through a 200 mesh sieve. ,

When this ground solid coke is mixed with the same mass, amount of fuel oil, the resulting slurry is a non-Newtonian liquid having a viscosity of 20.5 Pa.s at 93.3 ° C as measured by a Viscosimeter at 6 rpm and 12, 1 Pa.s. at 60 rpm.

In previous. In the examples, a laboratory-sized autoclave was used in which monolayers of material were processed. It goes without saying that any autoclave of known type can withstand pressures and temperatures that can be used in the process of the invention.

It will also be appreciated that although the foregoing description relates to single-feed autoclaves, the process of the present invention may employ relatively high-pressure autoclaves to which the feed is fed into the reactor inlet through a suitable closed hopper or other valve assembly, and the produced coke is withdrawn from the reactor cooling zone through a similar pressure outlet or valve orifice.

Although the invention has been described in accordance with specific examples, it will be appreciated that it can be varied and varied in various ways.

Claims (4)

1. A process for producing fuel from cellulosic materials, characterized in that the batch is heated in an autoclave at a temperature of 400 to 677 [deg.] C. at a pressure of 7 to 23 MPa, the water and the volatile organic components are converted into a gas phase. the batch composition and the resulting solid coke product is cooled and optionally ground. 2. Process according to claim 1, characterized in that, before the reaction product is cooled, the gas phase is discharged from the reactor and a condenser t is left, the non-condensable components being removed as gaseous effluents. 3. The process of claim 1 wherein the coke is ground to a particle size of less than 48 mesh and suspended in the fuel oil at a level of from about 1 to about 50 weight percent. % of coke, calculated on the total density of the liquid heating slurry. 4. Process according to claim 1, characterized in that cellulose from the group comprising tomato, agricultural waste, wood waste and their waste is used as the batch.