Title of Invention | "AN EQUIPMENT FOR THE PRODUCTION OF ACTIVATED CARBON FLEXIBLE MATERIALS USEFUL FOR ARRESTING POLLUTANTS" |
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Abstract | An equipment for the production of activated carbon flexible materials useful for arresting pollutants, containing roller drives for providing continuous feed of flexible material to a treatment chamber having conventional for heating and also controlling the pH an air drying non corrosive chamber being placed so as to accept the output of the said treatment chamber ,another roller drive being provided so as to allow continuous movement of the said flexible material through a bottom enclosure the said enclosure being connected to a heating reactor having heating elements in a furnace for providing a plurality of heat zones, the said heating reactor having a set of baffles being connected to a cooling chamber by flexible bellows , the said heating reactor and cooling chamber having ports for providing gaseous atmosphere at positive pressure, an outlet for exhaust gases produced being provided at the bottom portion of the said reactor at the outlet of the said cooling chamber roller drives being provided for effective continuous movement of the flexible material |
Full Text | The present invention relates to an equipment for the production of activated carbon flexible materials useful for arresting pollutants In the present context of global awareness and consequent action to bring down pollution in all spheres, it is very important to provide suitable materials which are useful for arresting pollutants. The process of preparing activated carbon from cloth has been described in an Indian patent (#175522 July 1995). The said patent is a laboratory demonstration of the treatment of a rayon cloth showing the effect of the processing parameters on the pores size and the effective surface area . The said patent uses the step of treating the cloth with organic solvents for initial cleaning for removing the impurities .The time periods used has been in the range of 1-24 hours. The next essential step described in the said patent is that of carbonisation and then separately of activation. In another patent (#US4256607) the oxidation of acrylonitrile based fibre has been done in a temperature range of 200 -300° C separately. Subsequently the oxidised fibre is activated from 700-1000° C for ten minutes to three hours. Both the above noted processes are essentially batch processes. To the best of our knowledge the equipment of the present invention is not in use in any industrial production line of textile mills, paper and printing etc The main objective of the present invention is to provide an equipment for the production of activated carbon flexible material use full for arresting pollutants and a process thereof. Another object of the present invention is to provide a treatment plant capable of treatment of the flexible material at a controlled temperature and at controlled pH. Yet another object of the present invention is to provide a heating reactor capable of effecting carbonisation and activation of the flexible material in a single reactor. Still another objective of the present invention is to provide a process for the production of activated carbon flexible material. In the drawing accompanying this specification figure 1 represents the total plant capable of producing the activated carbon flexible material wherein (1) is a set of roller drives to translate the material (2) to a treatment chamber (3). The treatment chamber has a means for heating the chemical used for treating the material and also has a set of roller to translate the material to a drying chamber (4). The heating reactor (6) receives the treated and dried material from drive (5) for carbonization and activation. The heating reactor contains gas inlets (7) and (8) and outlet (9). These gas inlets are used for feeding inert and activating gases and the outlets are used for the exhaust of gases. Connected to the heating chamber are metallic bellows (10) which are further connected to a cooling chamber (11) to receive the activated carbon flexible material. The heater reactor used in the present invention consists of a furnace (12) containing heating elements (13). The activation and carbonization takes place in a chamber (6) having a bottom enclosure (14). The chamber (6) is divided internally into two parts by means of baffles (15). Accordingly the present invention provides an equipment for the production of activated carbon flexible materials useful for arresting pollutants, which comprises: a) roller drives (1,2) for providing continuous feed of flexible material to a treatment chamber (3) having conventional for heating and also controlling thepH b) an air drying non corrosive chamber (4) being placed so as to accept the output of the said treatment chamber (3) c) another roller dries (5) being provided so as to allow continuous movement of the said flexible material through a bottom enclosure (14), characterized in that the said enclosure (14) being connected to a heating reactor (6) having heating elements (13) in a furnance (12) for providing a plurality of heat zones, the said heating reactor (6) having a set of baffles (15) being connected to a cooling chamber (11 by flexible bellows (10), the said heating reactor (6) d) at the outlet of the said cooling chamber (11) roller drives being provided for effective continuous movement of the flexible material. In an embodiment of the present invention means such as roller drives may be used powered by prime movers such as electrical motors having speed control means such as thyuristor drives. In another embodiment of the present invention means for heating in the treatment chamber may be such as an oil bath having heating means. In yet another embodiment of the present invention means for the pH control in the treatment chamber essentially consists of a pH monitor and a controlled supOply o water and/or treatment solution to maintain the pH. In still another embodiment of the present invention the plurality of heating zones in the heating reactor may be provided by using a plurality of external heating elements capable of prviding gradual heating at the rate of l°C/min to 10° C/min and maintaining a p0lurality of heat zones of temperature in the range of room temperature to 1000°C. In another embodiment fo the present invention means for providing the gaseous atmosphere in the beating reactor and cooling chamber may consist of separate inlet for each gas and common outlet for exhaust gases. In yet another embodiment of the present invention the gas inlet for the heating reactor may consist of an extended pipe inside the furnance in such a manner so as to enable the gas to be preheated. Accordingly the present invention provides a process for the production of activated carbon flexible material suing the equipment of the present invention, which comprises: a) treating a continuously fed flexible material at the speed in the range of 5-100 cm/hour with an oxidising agent having concentration in the range of 1-10 % and pH in the range of 0.1 to 2.0 at a temperature in the range of 50- 95 °C b) passing the said treated flexible material through a drying chamber maintained at a temperature in the range of 50- 200°C for a residence period of at least 30 minutes; c) passing the said treated and dried flexible material through a heating reactor to effect carbonisation and activation by providing plurality of increased temperature heating zones in the range of room temperature to 1000 °C arrived at by gradual heating at the rate of 1 °C/min to 10 °C/min in the presence of a mixture of inert and activation gases at a positive pressure; d) cooling the resultant activated carbon flexible material in an inert atmosphere. In an embodiment of the present invention the flexible material used may be such as viscose rayon cloth, felt , paper. In another embodiment of the present invention the oxidizing agent used may be such as orthophosphoric acid, zinc chloride ,potassium hydroxide. In yet another embodiment of the present invention the inert gas used may be such as nitrogen, helium or mixture thereof. In yet another embodiment of the present invention the activating gases used may be such as CO2, NH3, steam. In still another embodiment of the present invention the flow rate of inert and activating gases may be in the range of 5-1001it/min In another embodiment of the present invention the purity of inert and activating gases may be in the range of 90-99.5% pure. The equipment of the present invention essentially consists of drives for pulling and feeding the material to be activated . The drives are located in the initial feeding station, after the drying chamber serving as the feeder to the reactor and at the end of the reactor for pulling the activated material. The drives are fixed in such a way that by changing the speed of the drive the shrinkage and the residence time of the flexible material can be taken care of. The tension of the flexible material can also be adjusted accordingly. The pre- treatment chamber can be of any convenient shape and any non corrosive material. The dimensions of the treatment chamber are of suitable value for the convenience of erection . By adjusting the level of the treatment solution and the speed of the drive the material can be treated in the chamber for different intervals. There is a facility to heat the treatment solution by suitable means provided external to the chamber. There is a facility for monitoring the pH and the temperature of the treatment solution. The chamber meant for drying the pre-treated flexible cloth is also made of non corrosive material of any suitable size and geometry. The air meant for drying, blows in the chamber through a set of heaters installed in a suitable enclosure. The fumes so generated are sucked and diluted in an exhaust tank placed outside the equipment area. The main component of the equipment of the present invention is the heating reactor for effecting carbonisation and activation of the flexible material. The reactor is an air tight chamber heated by heating elements such that the chamber is heated from room temperature till 1000°C at a desired rate of heating, and can be maintained at the said temperature for a long time with a constancy of ±5°C. The material of the reactor chamber is of a suitable high temperature resistant and non corrosive material. In the bottom of the chamber a provision is made for feeding the treated and dried cloth. The chamber is divided into two parts by baffles. In the chamber there is a facility to provide hot gas at the reaction zone. A facility is also provided to suck the waste gases by controlled flow so that the positive pressure is always maintained in the chamber. A suitable device is fixed external to the reactor chamber for measuring the pressure. The top of the reactor chamber is connected to a cooling l' tower with a set of flexible bellows . This is required to take care of the expansion /contraction of the chamber due to high temperature differentials. In the cooling tank the activated flexible material is cooled in inert atmosphere. The cooling tower and the bellows are also of non corrosive material and of any convenient shape and size for ease of erection and commissioning. There is a top enclosure attached to cooling tower for coiling the flexible material. The main process of the present invention for the production of the activated carbon flexible material is described hereunder. Initially typically a viscose rayon cloth of approximately 10 meters length was taken on the first feed roller. The cloth was fed to the pre treatment chamber for chemical treatment in a suitable oxidising agent maintained at a temperature in the interval of 97+ 3°C. The treatment was done for a period of at least 1 hour. The pre-treated material was fed continuously to the drying chamber maintained at a temperature of 97 ± 3 °C . The drying was done for a period of at least 30 mins . Thedried material was collected on a drive feeder. Next the treated and dried material was stacked in a bottom enclosure of the reactor such that one end of the material is connected to the drive fixed on the top enclosure. The temperature of the reactor is raised approximately at the rate of 3 -8° C/hr. till a temperature of 1000° C and simultaneously the cloth is pulled approximately at the rate of 25-80cm/hr. Pulling of the material is done till end of the material is reached The temperature is maintained at 1000°C throughout the run. During the pulling process, gases are flown into the reactor at the desired places with the desired flow rates for effecting carbonisation and activation . The exhaust of the gases are maintained such as there is a positive pressure in the chamber. Tne following examples are given by way of illustrations of the equipment of the present invention and therefore should not be construed to limit the scope of the present invention. EXAMPLE -1 A viscose rayon cloth of density of 500gm/cc was taken. The total length of the cloth was 10 meters. The cloth was rolled on a feed roller . The feed roller was driven by an electrical motor with a speed reduction gear system .The speed of the feed to the treatment chamber was kept at 65 cm/hour. Treatment chamber was filled with 10% solution of orthophosphoric acid . The temperature of the solution was maintained at 97°C and the fluctuation in the temperature was 5°C and the pH was 0.5-0.9. The resident time in the chamber was lhr. After this the cloth was transported to the drying chamber maintained at a temperature of 97°C with a fluctuation of 5 °C. The drying time was 2hrs. The dried cloth was then collected on the driver roller fixed at the outlet of the drying chamber. After the drying sequence, the cloth was kept in the bottom portion of the reactor with one free end fixed on the third drive. The process of activation and carbonisation was started in this reactor by raising the temperature at a rate of 3-8°C /hr upto 850° C. The pulling of the cloth was done at the rate of 45 cm/hr. The carbon dioxide flow rate was maintained at 30 lit/min . The cloth was found burnt. EXAMPLE-2 ,f A viscose rayon cloth of density of 500 gm/cc was taken. The total length of the cloth was 10 meters. The cloth was rolled on a feed roller . The feed roller was driven by an electrical motor with a speed reduction gear system .The speed of the feed to the treatment chamber was kept at 65 cm/hour. Treatment chamber was filled with 10% solution of orthophosphoric acid . The temperature of the solution was maintained at 97 C and the fluctuation in the temperature was 5 °C and the pH was 0.5-0.9. The resident time in the chamber was Ihr. After this the cloth was transported to the drying chamber maintained at a temperature of 97 °C with a fluctuation of 5 °C. The drying time was 2hrs. The dried cloth was then collected on the driver roller fixed at the outlet of the drying chamber. After the drying sequence, the cloth was kept in the bottom portion of the reactor with one free end fixed on the third drive. In this case the reactor was made air tight to prevent burning of the cloth. The process of activation and carbonisation was started in this reactor by raising the temperature at a rate of 3-8 °C /hr up to 850 ° C. The pulling of the cloth was done at the rate of 30 cm/hr. The carbon dioxide flow rate was maintained at 20 lit/min and additionally nitrogen was flown at a rate of 20 lit/min. The cloth was found stiff and brittle EXAMPLE -3 A viscose rayon cloth of density of 450gm/cc was taken. The total length of the cloth was 10 meters. The cloth was rolled on a feed roller . The feed roller was driven by an electrical motor with a speed reduction gear system .The speed of the feed to the treatment chamber was kept at 65 cm/hour. Treatment chamber was filled with 5% solution of orthophosphoric acid . The temperature of the solution was maintained at 86 ° C and the fluctuation in the temperature was 5°C and the pH was 1.4-1.5. The resident time in the chamber was lhr. After this, the cloth transported to the drying chamber maintained at a temperature of 97°C with a fluctuation of 5 °C drying time was 2hrs. The dried cloth was then collected on the driver roller fixed at the outlet of the drying chamber. After the drying sequence the cloth was kept in the bottom >•-' portion of the reactor with one free end fixed on the third drive. The reactor was made air tight to prevent burning of the cloth. The process of activation and carbonisation was started in this reactor by raising the temperature at a rate of 3-8°C /hr upto 850 °C.The pulling of the cloth was done at the rate of 30 cm/hr. The carbon dioxide flow rate was maintained at 20 lit/min and nitrogen was flown at a rate of 20 lit/min. The cloth was found to be just flexible. EXAMPLE-4 A viscose rayon cloth of density of 350 gm/cc was taken. The total length of the doth was 10 meters. The cloth was rolled on a feed roller . The feed roller was driven by an electrical motor with a speed reduction gear system .The speed of the feed to the treatment chamber was kept at 65 cm/hour. Treatment chamber was filled with 5% solution of orthophosphoric acid . The temperature of the solution was maintained at 86 ° C and the fluctuation in the temperature was 5 ° C and the pH was 1.4-1.5. The resident time in the chamber was Ihr. After this, the cloth was transported to the drying chamber maintained at a temperature of 97 ° C with a fluctuation of 5 ° C drying time was 2hrs. The dried cloth was then collected on the driver roller fixed at the outlet of the drying chamber. After the drying sequence the cloth was kept in the bottom portion of the reactor with one free end fixed on the third drive. The reactor was made air tight to prevent burning of the cloth. The process of activation and carbonisation was started in this reactor by raising the temperature at a rate of 3-8 ° C /hr up to 850 °C. The pulling of the cloth was done at the rate of 30 cm/hr. The carbon dioxide flow rate was maintained at 20 lit/min and nitrogen was flown at a rate of 20 lit/min. The cloth was found to have improved flexibility. EXAMPLE -5 A viscose rayon cloth of density of 450gm/cc was taken. The total length of the cloth was 10 meters. The cloth was rolled on a feed roller . The feed roller was driven by an electrical motor with a speed reduction gear system .The speed of the feed to the treatment chamber was kept at 45 cm/hr., treatment chamber was filled with 10% solution of orthophosphoric acid. The temperature of the solution was maintained at f-s~ 86 OC and the fluctuation in the temperature was 5°C and the pH was 0.8-1. The residence time in the chamber was one hour . After this the cloth was transported to a drying chamber maintained at the temperature of 97 °C with the fluctuation of 5° C , the drying time was 2hrs. The dried cloth was then collected on the drive rollers fixed at the outlet of the drying chamber. After the drying sequence the cloth was kept in the bottom portion of the reactor with one free end fixed on the third drive. The reactor was made air tight to prevent burning of the cloth. The process of activation and carbonisation was started in this reactor by raising the temperature at a rate of 2-10°C /hr up to 1000° C. The pulling of the cloth was done at the rate of 20 cm/hr. The carbon dioxide flow rate was maintained at 15 lit/min and additionally nitrogen was flown at a rate of 15 lit/min. The cloth was found to have desired properties such as flexibility, yield and surface area. The main advantages of the present invention are: 1. The equipment is very simple to operate. 2. The equipment has a modular structure having the ease of maintenance and replacement of any defective parts. 3. The equipment can be used for semi- commercial production of Activated carbon flexible materials. 4. The equipment can be scaled up for a complete commercial plant. 5. The activated carbon flexible material produced by the process of the said invention has very unique properties of excellent flexibility yield and surface area.The process of producing the activated carbon flexible materials is very cost effective. 6. The process can be transformed very easuy for continuous production of activated carbon flexible materials with only minor changes. We Claim: 1. An equipment for the production of activated carbon flexible materials useful for arresting pollutants, which comprises: a) roller drives (1,2) for providing continuous feed of flexible material to a treatment chamber (3) having conventional for heating and also controlling the pH b) an air drying non corrosive chamber (4) being placed so as to accept the output of the said treatment chamber (3) c) another roller dries (5) being provided so as to allow continuous movement of the said flexible material through a bottom enclosure (14), characterized in that the said enclolzer (14) being connected to a heating reactor (6) having heating elements (13) in a furnance (12) for providing a plurality of heat zones, the said heating reactor (6) having a set of baffles (15) being connected to a cooling chamber (11 by flexible bellows (10), the said heating reactor and cooling chamber having ports (7), (8) for providing gaseous atmosphere at positive pressure, an outlet (9) for exhaust gases produced being provided at the bottom portion of the said reactor (6) d) at the outlet of the said cooling chamber (11) roller drives being provided for effective continuous movement of the flexible material. 2. An equipment as claimed in claims wherein the plurality of the heating zones gradual heating at the rate of 1 C/min to 10°C/min and maintaining a plurality of heat zones of temperature in the range of room temperature to 1000°C. 3. An equipment as claimed in claims wherein the ports consists of separate inlet for each gas and common outlet for exhaust gases. 4. An equipment as claimed in claims 3 wherein the gas inlet for the heating reactor consists of an extended pipe inside the said reactor so as to enable the gas to be preheated. 5. A process for the production of activated carbon flexible material using equipment as claimed in claim 1 which comprises : a) treating a continuously fed flexible material at a speed in the range of 5-100 cm/hour with an oxidizing agent selected from orthophosphoric acid, zinc chloride, potassium hydroxide having concentration in the range of 1-10%and pH in the range of 1.0-2.0 at a temperature in the range of 50-95°C, b) passing the said treated flexible material through a drying chamber maintained at a temperature in the range of 50-200°C for a residence period of at least 30 minutes, c) passing the said dried treated flexible material through a heating reactor to effect carbonization and activation by providing plurality of increased temperature heating zones in the range of room temperature to 1000°C arrived at by gradual heating at the rate of l°C/min to 10°C/min in the presence of a mixture of inert and activation gases selected from nitrogen,helium or mixture thereof at a positive pressure, d) cooling the resultant activated carbon flexible material in an inert atmosphere. 6, An equipment for the production of activated carbon flexible materials useful for arresting pollutants substantially as herein described with reference to the example; and the drawing accompanying this specification |
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447-del-1999-correspondence-others.pdf
447-del-1999-correspondence-po.pdf
447-del-1999-description (complete).pdf
Patent Number | 231523 | ||||||||||||||||||||||||||||||
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Indian Patent Application Number | 447/DEL/1999 | ||||||||||||||||||||||||||||||
PG Journal Number | 13/2009 | ||||||||||||||||||||||||||||||
Publication Date | 27-Mar-2009 | ||||||||||||||||||||||||||||||
Grant Date | 05-Mar-2009 | ||||||||||||||||||||||||||||||
Date of Filing | 19-Mar-1999 | ||||||||||||||||||||||||||||||
Name of Patentee | COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH | ||||||||||||||||||||||||||||||
Applicant Address | RAFI MARG,NEW DELHI 110001 | ||||||||||||||||||||||||||||||
Inventors:
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PCT International Classification Number | C01B 31/08 | ||||||||||||||||||||||||||||||
PCT International Application Number | N/A | ||||||||||||||||||||||||||||||
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