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INVENTION
Russian Federation Patent RU2118291

METHOD FOR CONTINUOUS carboniferous raw materials processing
AND DEVICE FOR ITS IMPLEMENTATION

Name of the inventor:
The name of the patentee: Limited Liability Company "plow"
Address for correspondence:
Starting date of the patent: 1998.02.26

The invention relates to the preparation of active carbon from a carbonaceous feedstock. The method comprises the steps of preheating the carbonaceous feedstock to a temperature of ^120-150 o C, carbonization and activation, and supplying the resulting vapor mixture in countercurrent to the solid carbonized carbonaceous feedstock recycling process is carried out in the absence of oxygen by feeding dry nitrogen countercurrently to the solid carbonation step preheating raw materials and / or carbonization is carried out in the presence of additives halogen or metal halide or ammonium halide or mixtures thereof and a sulfur-containing reagent carbonization process is carried out at temperatures from 150-250 to ^600-700 o C, formed into a preheating stage of raw carbonizing the gummy product was separated and solid carbonization product from the activation stage is sent to the cooling step while moving the solid carbonization product at each stage of the conversion process is performed forcedly, with an adjustable speed of movement, the active carbon having the maturation stage is discharged and the steam-gas mixture formed on the maturing stage is sent to the previous stage, the gas-vapor mixture is withdrawn from the refining process of raw materials prior heating step and directed to separation and isolation of aqueous-organic resinous condensation product. Thus halogen or metal halide or ammonium halide, or a mixture thereof is administered in an amount of 0.5-1 wt.%, A sulfur-containing agent is administered in an amount of 5.4 wt.% Based on sulfur, the activation is carried out with superheated steam. The process is carried out in an apparatus comprising serially connected by downcomers nozzle and arranged one below the other preheating chamber, carbonization and activation, the feed components, superheated steam and outlet of active charcoal, an outlet for removing the vapor-gas mixture supply reactive additives node processing process, ripening chamber with a nozzle for input of dry nitrogen, connected in series via the overflow pipe with the camera activation and placed under it, and the block division of the gas-vapor mixture with spigots O resinous product and aqueous-organic condensate, whose input is connected to a nozzle for discharging the gas-vapor mixture, placed in the top preheating chamber portion. In this chamber are in the form of identical reactors, screw-type actuators, pre-heating and carbonization chamber are heating shirt, activation and maturation of the chamber - cooling jacket and activated carbon removal unit is placed on the maturation of the chamber outlet. The invention enables an integrated process for the low-temperature carbonaceous feedstock technology obtain activated carbon with enhanced adsorption capacity for crude oil and petroleum products and additional organic resins and organic condensate.

DESCRIPTION OF THE INVENTION

The invention relates to the production of active carbon and organic products from carbonaceous materials, preferably ligninuglevodistogo.

Activated carbon recycling process can be used to collect oil spills, soil cleaning process solutions, industrial wastewater, water bodies and objects of environmental disasters.

A method of processing carbonaceous materials (wood, lignin tsellolignina, coal, etc.), comprising carbonizing materials in a rotary kiln at a rate rise ^15-40 o C / min to a temperature of ^400-650 o C in an atmosphere of carbon dioxide or flue gases. Carbonized product was discharged, cooled and fed into another reactor where heating is performed without access of gaseous reactants to ^800-850 o C at a temperature of ^50-100 o C / h Pumping rate. Then, without cooling the steam activated product. Upon completion of the activation process the active carbon is discharged, cooled and shredded. (Patent RF N 2023661, C 01 B 31/08, 1994).

A disadvantage of the known method consists in the sophisticated technology of the process involves the use of high temperatures.

Known method, and continuous processing of carbonaceous materials in an apparatus for producing active coal in a fluidized bed, comprising the step of preheating the raw material at a temperature of ^100-150 o C, the low-temperature carbonization at a temperature of ^400-500 o C, carbonization at high temperature ^750-850 o C activation solid carbonization gas-vapor mixture. (Avt.svid. USSR N 467761, C 01 B 31/08, 1970).

Steam-gas mixture formed in the combustion chamber during combustion (here serves as steam) is passed successively upwards through the activation chamber, high-temperature carbonization, the low-temperature carbonization and preheating feedstock countercurrent to the solid carbonation. Ready activated carbon is removed from the process with the activation step.

A device for continuous processing of carbonaceous materials containing serially connected by downcomers pipes and placed one under the other reactionary preheating the low-temperature and high-temperature carbonization and activation of the camera, the feed components and superheated steam pipes to remove the active coal and gas mixture. (Ed.'s Certificate. USSR N 467761, C 01 B 31/08, 1972).

The disadvantages of the known method and apparatus are complicated technology of the process with the use of high temperatures, the preparation of activated carbon with a low sorption capacity with respect to oil and petroleum products and nedoizvlechenie organic processed products due to the limited technological capabilities.

The object of the invention to provide a method and apparatus for its implementation which allow the complex to process carbonaceous feedstock by simple low temperature techniques to produce an active carbon having a higher sorption capacity for oil and oil products, and further processing of products - resins and organic condensate.

The task is achieved by a method of continuous processing of carbonaceous materials comprising the steps of pre-heating the raw material to a temperature of ^120-150 o C, carbonization and activation, and the resulting gas mixture flow countercurrent to the solid carbonization feedstock according to the invention prior heating step and / or carbonization in the presence of additives are halogen, metal halide or ammonium halide or mixtures thereof and a sulfur-containing reagent carbonization process is carried out at temperatures ranging from 150-250 to ^600-700 o C, the resulting raw material into a preheating stage of carbonization and the gummy product was separated, and the solid carbonization to activation step is sent to an additional step of maturation, which serves dry nitrogen countercurrently to the solid carbonization while the movement of the solid carbonization product at each stage of the recycling process is carried out forcibly at a controlled speed of movement, the active carbon having the maturation stage is discharged and formed on maturation stage steam-gas mixture is sent to the previous stage, the gas-vapor mixture is withdrawn from the refining process of raw materials prior heating step and directed to separation and isolation of aqueous-organic resinous condensation product.

And the fact that:

- A halogen, metal halide or ammonium halide or a mixture thereof is administered in an amount of 0.5-1 wt.%;

- Sulfur-containing agent is administered in an amount of 5.4 wt% based on sulfur;.

- Activation is carried out with superheated steam.

The task is achieved by the fact that the device for the continuous processing of carbonaceous materials comprising serially connected by downcomers nozzle and arranged one below the other preheating chamber, carbonization and activation, the feed components, superheated steam and outlet of active charcoal and an outlet for removing the vapor-gas mixture according to the invention is provided with a unit supplying reactive additives during processing chamber maturation with a socket for input of dry nitrogen, serially connected by means of the overflow pipe with a camera activation and placed under it, and the block separation gas mixture with spigots O gummy product and aqueous-organic condensate input which is connected to the nozzle for discharging the gas-vapor mixture, placed on top of the pre-heating chamber, wherein the chambers are in the form of identical reactors, screw-type actuators, the preheating chamber and carbonization are heating jacket, activation and maturation chamber - cooling jacket and retraction assembly activated carbon available on the maturation of the chamber outlet.

And the fact that:

- Activated carbon removal unit is designed as a gateway discharge gate;

- The source of superheated steam is connected to activate the camera;

- Screw reactor provided with a variable pitch along the length of the screw shaft;

- At least one screw of each screw is formed with a slope opposite to the slope of the remaining screws;

- Screw auger is made for at least four slots;

- Feed unit is designed as a feeder-hopper, in the lower part of which is placed an inclined screw conveyor, connected via a gateway to the charging port preheating chamber;

- A cavity-feeder hopper agitator connected to the drive;

- Feed additives reaction unit is connected to the input hopper-feeder and / or to the input of the carbonation chamber;

- Inclined to the cavity the feed screw assembly connected pipe conveyor for feeding dry nitrogen;

- On the weekends areas preheating and carbonation cameras installed fittings resin relief, cameras are equipped with bumpers solid carbonization products installed on their ends.

FIG. 1 is a diagram of the proposed device; FIG. 2 - auger screw reactor;
FIG. 3 - A-A sectional view in Figure 2.

An apparatus for continuous processing of carbonaceous materials consists (Fig. 1) of the preheating chambers 1, 2 carbonization, activation, and maturation 3 4. Chambers are in the form of identical screw-type reactors, which screw shafts 5, 6, 7, 8 are respectively connected to actuators 9, 10, 11, 12. Chambers 1, 2, 3, 4 are arranged below each other and are connected in series between a nozzle through downcomers 13, 14 and 15.

preheating chambers 1 and 2 have carbonation electrical heating jacket 16, 17, and activation and maturation chamber 3 4 - cooling jacket 18, into which water entering through fitting 19, and the output - via the connection 20.

To activate the camera 3 via the nozzle 21 is carried out supply of superheated steam from the steam generator 22. The camera is connected via 4 maturation fitting 23 to 24 nitrogen units.

Feed of raw material for processing through feedstock supply unit 25 which consists of a hopper-feeder 26 and the inclined screw conveyor 27 to a pipe 28 feeding dry nitrogen to exclude air from entering from the atmosphere.

The angle of inclination of the screw conveyor 27 is chosen on the basis of conditions to ensure the efficiency of reagent supply with raw materials for the processing chain.

In the cavity of the hopper-feeder 26, an agitator 29 connected to the drive 30. Loading of raw materials in the feed hopper 26 is made through the nipple 31 and the preheating chamber 1 via a gateway charging port 32. Discharge of activated carbon from the device via the discharge unit 33, formed as a discharge sluice hatch.

Performing raw boot components and discharging activated carbon in the form of the sluice hatches provides a recycling process in holding anoxic environment by eliminating the ingress of oxygen from the environment into the reaction zone. The apparatus comprises a unit supplying reactive additives 34 (halogens, metal halides, or ammonium or a mixture thereof and a sulfur-containing reagent) in the recycling process, which is connected to the nozzle 35 of the feeder hopper 26 and / or to connecting pipes 36 and 37 enter halides and sulfur-containing carbonization chamber Reagent 2 .

Retraction vapor mixture produced from the process of refining the preheating chamber 1 through the pipe 38 which is connected to the input gas mixture separation block 39. The output from the last aqueous-organic resinous condensation product and is carried out respectively through nozzles 40 and 41.

At the ends mounted cameras 1-4 chippers solid carbonation 42, and output sections of the preheating chambers 1 and 2 are set carbonization resin relief fittings 43, 44 to prevent coking and carbon contamination of the final products of coking.

1-4 augers reactors (2) are variable-pitch propellers 45 along the length of the rolls 5-8, and at least one screw is formed with a slope opposite to the slope of the remaining screws. When this screw augers 45 carried by at least 4 of the groove 46 (Figure 3). This design provides optimal performance conditions augers move materials and reaction products at each stage of the process and eliminates formation of stagnant zones. separation unit 39 and camera 47 equipped with a thermocouple 1-4 for temperature control.

The process is performed as follows: the prepared ligninuglevodistoe raw materials (lignin, any waste of wood, cellulose, and others.) With optimal humidity of about 20 wt. % Comes from the hopper-feeder 26 by conveyor 27 through the airlock loading hatch 32 into the preheating chamber 1. Here from feed unit 34 via the connection 35 of the feeder hopper 26, and then the gateway charging port 32 simultaneously with the feedstock is fed ligninuglevodistym reaction additives - halogen halides of alkali or alkaline earth metal (e.g., chlorides or fluorides of sodium, potassium, calcium) or ammonium halides, or mixtures thereof and a sulfur containing reactant S ^0, HS ^-, S ^-2 ions is not less than 95 wt% (eg. elemental sulfur, sulfides, zinc sulfides oil). Reaction feed additives in feedstock ligninuglevodistogo processing can be performed in the carbonization chamber 2 via the nozzles 36 and 37 at the same time or in the preheating chamber 1 and feed the carbonization chamber 2. The halogen or metal halide or ammonium halide, or mixture thereof advantageously introduced into the process in an amount . 0.5-1 wt%, and a sulfur-containing agent - in an amount of 4.5% based on the sulfur.

In the preheating chamber 1 while moving along the screw feed is a thermochemical treatment at a temperature of ^120-150 o C with the occurrence of dehydration reactions dehydroxylation and partially sulfonation. The residence time of feedstock in the first stage, and a stage of carbonization, activation, and maturation of selected depending on the type and quality of used materials and additives, and the time spent in each chamber set screw moving speed. The resulting raw material prior to the heating step resinous product is further discharged through the nozzle 43, and the gaseous products formed in the flow of water vapor and nitrogen, the latter coming from the chambers 2, 3, 4, enter the separation unit 39.

The treated solid is heated and down-flow pipe 13 enters the carbonization chamber 2, where when moving the auger occurs by thermochemical decomposition (catalytic sulfonation, decarboxylation) in the range of temperatures from 150-250 to ^600-700 o C. gum-like product formed in step carbonization is withdrawn further via the connection 44, the gaseous products enter the chamber, together with one of the gaseous products below the reactors.

The solid product carbonization down-flow pipe 14 enters into the activation chamber 3, which is fed through the nozzle 21, superheated steam. With stirring at a temperature of 150-250 auger ^o C, the product is steamed to a temperature T i 180 ^o C. As a result of the hydroxylation process of the gaseous products formed enter the chamber 2, which are involved in the catalytic solid sulfonation, the resulting solid product A down-flow pipe 15 4 enters the ripening chamber.

During the movement of the solid product by carbonization in the screw ripening chamber 4 is its maturation and drying excess moisture from the dry nitrogen countercurrent (membrane nitrogen) supplied through the nozzle 23. The excess moisture in the form of vapor and nitrogen gas to enter an upper chamber 3, 2, 1. The product at the outlet chamber 4 is a trademark active carbon at a temperature ^40-45 o C, it is discharged under nitrogen through a sluice hatch retraction assembly 33 and via the scraper conveyor is transferred to a product silo (not shown in Figure 1).

nitrogen in the feed raw material feeding unit 25 and ripening chamber 4 provides a process flow in an oxygen-free environment, which provides an activated carbon with reproducible properties in each recycle process. The gaseous products of all the reactors are removed from the feedstock preheating chamber 1 into the separation unit 39. The separation unit 39 emit resinous material which is discharged via the nozzle 40, and aqueous-organic condensate (water, organic acids, alcohols, turpentine, and other organic compounds), which outputted via the connection 41.

The resin was collected in a tank and implement as a commercial product, and aqueous-organic condensate was collected in the container and sent for further processing as a raw material for the chemical industry.

Example 1. The prepared wood chips with a moisture content of about 20 wt. % In an amount of 722 kg / h, and the reaction agent (powdery ammonium chloride - 8 kg / h, powdered sulfur - 40 kg / h) fed to raw material preliminary heating chamber 1. In this chamber the raw materials in the presence of additives, by auger moving for 30 minutes at a temperature of 230 ± 10 ^o C, loses moisture (144 kg) and subjected to processes of dehydration and dehydroxylation partially sulfonation. The resulting gaseous products in the vapor stream and the nitrogen coming from the subsequent chambers 2, 3, 4 in total 578 kg enter the separation unit. The solid product in an amount of 578 kg / hr enters the carbonization chamber. Carbonization temperature of 230 to ^600-700 o C. The time for passage of the screw reactor 30 min. The solid product after thermochemical degradation in an amount 398 kg / h falls out into the activation chamber 3. The total amount of exhaust gases based on receipt of a gaseous phase downstream of the chambers 3 and 4 is 434 kg / h.

The activation chamber 3 carbonisation solid product in an amount of 398 kg / h is treated with superheated steam at a temperature T i 180 ^o C, supplied in an amount of 45 kg / h. The residence time in the chamber 3-20 minutes. The resulting gaseous products enter the chamber 2 involved in the amount of about 50 kg / h in a catalytic sulfonation. The solid product in an amount of 333 kg / h in the chamber 4 falls out.

The chamber 4 is obtained activated carbon is dried membrane nitrogen from excess moisture and maturing. Nitrogen supply amount ^of 6 ^m3 / h.

Excess moisture in a vapor of 40 kg / h and nitrogen gas in an amount of 6 m ³ / h coming from the chamber 4 in an upper chamber 3, 2, 1. The resulting active carbon at a temperature ^40-45 o C is a commercial product and is transferred to the warehouse finished product.

The gaseous products from all the cameras in an amount of about 578 kg / h, including about 200 kg water / h to enter the separation unit.

The separation unit is isolated from the gas mixture 72 kg / h of resinous substances, 450 kg / h of aqueous-organic condensate comprising water, organic acid, alcohol, turpentine, et al., The residue of the gas phase in an amount of 48 m ³ / h discharged into the atmosphere. Yield of active carbon based on the dry substance of about 50 wt.%.

The main characteristics of the resulting activated charcoal:

• General Properties - black crystalline powder with a metallic sheen.
• Brinell hardness - 1-2
• Mechanical strength, kgf / cm ² - 10-15
• Density, kg / m ³ - 310 (bulk)
• Pressed density, kg / m ³ - 460 ± 10
• Size fractions, mm - 0.3-5
• Limit the volume of sorption to water vapor, cm ³ / g - 0.14
• Solubility in 1,5 NaOH (immersion), wt% -. 6 Before
• Porosity, pore volume in cm ³ / g - 0.2-0.4
• oil saturation time with - 5-10
• Secondary oil recovery for 24 hours (water)% - 0,0008-0,0015
• Natural humidity,% - 3-4
• Yield on dry matter,% - 50
• Capacity hard granular sorbent from the original volume - 0,85-0,8
• Toxicity - Non-toxic
• Operating temperature, ^o C - 20 ± 80
• Thermal stability, ^o C - 210 ± 10
• Traceability throughout the year - not observed
• Thermal conductivity, W / m ³W ^o C - 0.05-0.06
• Disposal of waste - non-waste in the construction industry.
• Resistance to acid, standard conditions - chemical degradation was observed.
• Field of use - collection of all kinds of oil, bitumen and oil from any surface, processing lyalnyh waters on tank farms, oil and fat, and others.

Examples of the method for different types of carbonaceous materials shown in Table additionally. 1 and 2.

Thus, the proposed method and device make it possible to obtain activated carbon with high sorption capacity for oil and oil products (see. The above-mentioned quality characteristics) for a simple continuous low-temperature technology, and obtain valuable organic and processed products.

CLAIM

1. A continuous process for refining carbonaceous feedstock, comprising pre-heating the raw material stage to a temperature of 120 - 150 ° C, carbonization and activation, and the resulting gas mixture flow countercurrent to the solid carbonation, wherein the feedstock preheating step and / or carbonization is carried out in the presence of additives halogen, metal halide or ammonium halide or mixtures thereof and a sulfur-containing reagent carbonization process is carried out in the temperature range of 150 - 250 and 600 - 700 ° C, formed into a preheating raw stages and carbonizing the gummy product was separated and solid carbonization with activation step is sent to an additional step of maturation, which serves dry nitrogen countercurrently to the solid carbonization while the movement of the solid carbonization product at each stage of the recycling process is carried out forcibly at a controlled speed of movement, after which the active carbon having the maturation stage is discharged and the resulting at step maturation steam-gas mixture is sent to the previous stage, the gas-vapor mixture is withdrawn from the refining process of raw materials prior heating step and directed to separation and isolation of aqueous-organic resinous condensation product.

2. A method according to claim 1, characterized in that the halogen or metal halide or ammonium halide, or a mixture thereof is administered in an amount of 0.5 - 1 wt.%.

3. The method of claim 1, wherein said sulfur-containing agent is administered in an amount of 4 -. 5 wt. % Based on the sulfur.

4. The method of claim 1, wherein the activation is carried out with superheated steam.

. An apparatus for continuous processing of carbonaceous materials comprising serially connected by downcomers nozzle and arranged one below the other preheating chamber, carbonization and activation, the feed components, superheated steam and outlet of active charcoal and an outlet for removing the vapor-gas mixture, characterized in that it is provided node supply reactive additives in the recycling process, ripening chamber with a nozzle for input of dry nitrogen, serially connected through the overflow pipe with the camera activation and placed under it, and the block division of the gas-vapor mixture with spigots O resinous product and vodoogranichennogo condensate, whose input is connected to the pipe for discharging the gas-vapor mixture, placed on top of the pre-heating chamber, wherein the chambers are in the form of identical reactors, screw-type actuators, the preheating chamber and carbonization are heating jacket, activation and maturation chamber - cooling jacket and active carbon removal unit placed on the output ripening chamber.

6. Apparatus according to claim 5, characterized in that the active carbon removal unit is designed as a discharge sluice hatch.

7. Apparatus according to claim 5, characterized in that the source of superheated steam connected to the activation chamber.

8. Apparatus according to claim 5, characterized in that the screws are made of reactors with variable pitch screws along the length of the shaft.

9. Apparatus according to claim 8, characterized in that at least one screw of each screw is formed with a slope opposite to the slope of the remaining screws.

10. The apparatus of claim 9, wherein said screw auger performed at least four slots.

11. Apparatus according to claim 5, characterized in that the feed unit is designed as a feeder-hopper, in the lower part of which is placed an inclined screw conveyor, connected via a gateway to the charging port preheating chamber.

12. The apparatus of claim 11, characterized in that the agitator drive connected to a cavity-feeder hopper.

13. The apparatus of claim 5, wherein said reaction feed additives node connected to the input hopper-feeder and / or to the input of the carbonization chamber.

14. The apparatus of claim. 11 wherein the cavity for the feed of the inclined screw conveyor assembly for feeding pipe connected dry nitrogen.

15. Apparatus according to claim 5, characterized in that the output plots preheating chambers and carbonization additionally installed fittings reset resin.

16. Apparatus according to claim 5, characterized in that the camera provided with the solid carbonization product bumpers mounted on their ends.

print version
Publication date 07.01.2007gg

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