WO2021038583A1 - Procédé autonome à une seule étape d'activation in situ pour la synthèse de charbon actif à partir de résidus agro-chimiques - Google Patents

Procédé autonome à une seule étape d'activation in situ pour la synthèse de charbon actif à partir de résidus agro-chimiques Download PDF

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Publication number
WO2021038583A1
WO2021038583A1 PCT/IN2020/050732 IN2020050732W WO2021038583A1 WO 2021038583 A1 WO2021038583 A1 WO 2021038583A1 IN 2020050732 W IN2020050732 W IN 2020050732W WO 2021038583 A1 WO2021038583 A1 WO 2021038583A1
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WO
WIPO (PCT)
Prior art keywords
activated carbon
activation
reactor
steam
synthesis
Prior art date
Application number
PCT/IN2020/050732
Other languages
English (en)
Inventor
Muthu Kumar K
Varunkumar S
Syed MUGHEES ALI
Original Assignee
INDIAN INSTITUTE OF TECHNOLOGY MADRAS (IIT Madras)
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by INDIAN INSTITUTE OF TECHNOLOGY MADRAS (IIT Madras) filed Critical INDIAN INSTITUTE OF TECHNOLOGY MADRAS (IIT Madras)
Publication of WO2021038583A1 publication Critical patent/WO2021038583A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B49/00—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated
    • C10B49/02—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated with hot gases or vapours, e.g. hot gases obtained by partial combustion of the charge
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/336—Preparation characterised by gaseous activating agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/39—Apparatus for the preparation thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B49/00—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated
    • C10B49/02—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated with hot gases or vapours, e.g. hot gases obtained by partial combustion of the charge
    • C10B49/04—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated with hot gases or vapours, e.g. hot gases obtained by partial combustion of the charge while moving the solid material to be treated
    • C10B49/06—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated with hot gases or vapours, e.g. hot gases obtained by partial combustion of the charge while moving the solid material to be treated according to the moving bed type
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
    • C10B57/12—Applying additives during coking
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
    • C10K1/101—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids with water only
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the present invention generally relates to biomass processing systems and methods.
  • the present invention is additionally related to activated carbon from agro residues.
  • the present invention also relates to combustion techniques for synthesis of activated carbon from agro residues.
  • the present invention specifically relates to a self-sustained single-step activation in situ process for activated carbon synthesis from agro residues.
  • FIG. 1 and FIG. 2 a two-step activated carbon production technique involving charcoal production (FIG. 1) and activated carbon production (FIG. 2) is proposed.
  • coconut shells lie
  • a mud pit (1 la)
  • This system consists of a mud pit (1 lh) into which coconut shells are loaded via port (8f).
  • the loaded coconut shells are ignited.
  • the limited supply of air required for the carbonization (or oxidative pyrolysis) is taken by natural convection into the mud-pit via port (Ilf).
  • the cooled charcoal from the stage one is further taken to the second stage for converting it to activated carbon.
  • the charcoal (12b) is loaded into the rotary kiln (12a) from one end.
  • the rotary kiln is maintained at a temperature of about 800°C by using the heat energy of the volatiles that is trapped inside the charcoal.
  • the heat energy from the charcoal is released by igniting the charcoal with limited supply of air.
  • the steam is also supplied into the rotary kiln (12c).
  • the steam (12c) is generated using a steam generator (12d) which is typically powered using diesel/electricity (12e).
  • the conventional prior art processes for production of activated carbon teaches a two-stage process which is inefficient and energy intensive.
  • the conventional prior art process is disadvantageous as the superheated steam and high temperature conditions (-750 °C) required for activation of charcoal to produce activated carbon (AC) is typically provided using fossil fuels (e.g., diesel).
  • fossil fuels e.g., diesel
  • one aspect of the disclosed embodiment is to provide for an improved process for production of activated carbon from agro residues.
  • a self-sustained single-step activation in situ process for activated carbon synthesis from agro residues is disclosed herein.
  • the invention teaches production of activated carbon (AC) in a single step by physical activation using steam as the activation agent.
  • the AC is produced in a continuous process in a fixed bed reactor directly from coconut shells without it being converted to charcoal and without using any external heat source.
  • the proposed method employs the heat of partial combustion of volatiles (generated during de-volatilization of coconut shells) to maintain the required temperature inside the reactor.
  • volatiles generated during de-volatilization of coconut shells
  • the hot products of oxidation of volatiles will pass through the char bed to maintain the temperature of the bed above 750 °C.
  • superheated steam of temperature around 200 °C will be passed through the char bed to convert it into activated carbon. Heat from volatile combustion is used for steam generation as well.
  • FIG. 1 and FIG. 2 illustrates a prior art two-step process 100 and 200 for production of activated carbon
  • FIG. 3 illustrates a batch type system 300 for the production of activated carbon, in accordance with the disclosed embodiments
  • FIG. 4 illustrates a self-sustained single-step activation in situ process 400 for activated carbon synthesis from agro residues, in accordance with the disclosed embodiments
  • FIG. 5 illustrates the activation unit 500 of the self- sustained single-step activation in situ process 400 for activated carbon synthesis from agro residues, in accordance with the disclosed embodiments
  • FIG. 6 illustrates the material handling unit 600 of the self-sustained single-step activation in situ process 400 for activated carbon synthesis from agro residues, in accordance with the disclosed embodiments;
  • FIG. 7 illustrates the material scrubber unit 700 of the self-sustained single-step activation in situ process 400 for activated carbon synthesis from agro residues, in accordance with the disclosed embodiments;
  • FIG. 8 illustrates the steam generation unit 800 of the self-sustained single-step activation in situ process 400 for activated carbon synthesis from agro residues, in accordance with the disclosed embodiments.
  • a self-sustained single-step activation in situ process for activated carbon synthesis from agro residues is disclosed herein.
  • the invention teaches production of activated carbon (AC) in a single step by physical activation using steam as the activation agent.
  • the AC is produced in a continuous process in a fixed bed reactor directly from coconut shells without it being converted to charcoal and without using any external heat source.
  • the proposed method employs the heat of partial combustion of volatiles
  • FIG. 3 illustrates a batch type system (300) for production of activated carbon and it consists of an activation reactor (a), steam generator (b), compressor (c), temperature monitoring unit (d), distributor plate or grate (e), LPG combustor (1), Thermocouples (m), a pump (g) and a sump (h).
  • a steam generator unit (b) for receiving water (t) from the bottom portion and the superheated steam (u) is removed from the top and is supplied into bottom of the reactor wherein the steam generator unit (b) is powered by
  • LPG combustor uses LPG j) as fuel.
  • a compressor(c) is used to supply air into the bottom of the reactor below the grate (e) where the temperature of the reactor is monitored using thermocouples connected to a Data acquisition system (d).
  • the coconut shells (o) are ignited at the top of the reactor under limited supply of air supplied from the compressor(c) wherein air is supplied from the bottom to the top of the reactor and is monitored using mass flow controller (cl).
  • the flame front/reaction zone (p) is initially established at the top of the reactor and starts to move towards the bottom leaving a hot char zone (q) above it.
  • the superheated steam (u) is supplied into the hot char zone for a specific period of time from the bottom of the reactor and a residence time of 2-3 hours is provided for the char to react with the steam inside the reactor for the char to get converted to activated carbon (r) wherein the temperature of the char zone in the presence of steam is maintained above 750 °C.
  • the temperature of the reactor is monitored using a temperature monitoring system (d) wherein the temperature of the hot char zone can be varied by varying the air supply rate.
  • the activated carbon is removed from the top of the reactor.
  • a continuous system consisting of an activation reactor (1), where coconut shells (li) are loaded from the top and supported on a grate (lb) at the bottom. The bed is ignited near the grate. A thin (4-5 times the particle thickness) high temperature reaction zone (lj) is established wherein the reaction zone generally propagates upwards after ignition.
  • FIG. 4 illustrates a self-sustained single-step activation in situ process 400 for activated carbon synthesis from agro residues, in accordance with the disclosed embodiments.
  • the system comprises a material handling unit (2) consisting of a coconut shell crusher (2a) for sizing the coconut shells before loading into the system 400, a slide gate valves (2b and 2c) to control the flow of activated carbon from the bottom of the reactor (lc), a screw conveyor (2d) and a collecting drum (2e) (fitted to the screw conveyor) for removing the material at a controlled rate and storing it respectively.
  • a material handling unit (2) consisting of a coconut shell crusher (2a) for sizing the coconut shells before loading into the system 400, a slide gate valves (2b and 2c) to control the flow of activated carbon from the bottom of the reactor (lc), a screw conveyor (2d) and a collecting drum (2e) (fitted to the screw conveyor) for removing the material at a controlled rate and storing it respectively.
  • the system comprises a scrubbing unit (3) to remove particulates and/or condensable vapors from the producer gas.
  • the scrubbing unit (3) has a scrubber tank (3 a).
  • the scrubber tank (3 a) has a mist eliminator (3b) and a nozzle arrangement (3c) to remove moisture and to supply water spray respectively to the producer gas.
  • Scrubber unit also has a water tank (3e) to store the water, a pump arrangement (3d) to circulate water through the scrubber.
  • the system 400 also has a blower (4a) to keep the reactor and the gas path under suction.
  • a flow measuring device (4c) is used to measure the flow rate of exhaust gas.
  • the system 400 includes has a burner-steam generator unit (5) wherein the exhaust gas coming from the reactor (lc) via the scrubber unit (3) and blower 4a) is burned in the exhaust gas burner (5 a).
  • the secondary air required for the burner (5a) is supplied through the port (5d) using a compressor (5e).
  • the flow rate of the secondary air is measured using a rotameter (5f).
  • the burned gases from the exhaust of the burner (5a) are supplied into the steam generator (5b) from its bottom via the gas inlet port (5g).
  • the water required for steam generation is supplied through the water inlet port (5h).
  • the water is pumped to the steam generator from the sump (5i) using a pump (5j).
  • a mass flow controller is used to control the flow rate of water.
  • Superheated steam is produced inside the steam generator (5b) and is removed from the steam exit port (51) and is passed into the reactor via steam inlet port lh) of the reactor (1).
  • the loaded coconut shells (li) are ignited at the bottom of the reactor under a limited supply of air sucked into the reactor via air inlet port (lg) using the blower (4a).
  • the flame front/reaction zone (lj) is initially established at the bottom of the reactor and starts to move from the bottom to the top leaving a hot char zone (lk) below it.
  • the superheated steam is supplied into the hot char zone for a specific period of time from the top of the reactor via steam inlet port (lh).
  • the temperature of the char zone in the presence of steam is maintained above 750 °C.
  • the temperature of the reactor is monitored using thermocouples (le) connected to the temperature monitoring system (lc).
  • the temperature of the hot char zone can be varied by varying the air suction rate.
  • the air suction rate through air inlet port (lg) can be controlled by varying the speed of the blower using variable frequency drive.
  • the air suction rate is indirectly measured by measuring the exhaust gas flow rate using the flow measuring device.
  • the producer gas (Id) coming out of the activation reactor (1) is passed through the scrubber unit (3) via scrubber inlet port (3f).
  • Pump (3d) is used to supply high pressure water to the nozzle (3c) which produces a fine spray in the counter-current direction to the producer gas (Id) flow in order to remove the particulates and/or condensable gases from the gas stream.
  • the water (3h) from the scrubber is drained out and collected back in the water collection drum (3e).
  • the cleanedgas (3g) is then passed into the exhaust gas burner (5) via the inlet port (5c) and is completely burned inside the burner.
  • the burned gas from the burner exhaust is sent into the steam generator (5b) via the hot gas inlet port (5g) for the generation of superheated steam which is supplied back into activation reactor (1) via steam inlet port (lh).
  • the scrubber can be improvised by adding a cyclone and a condensing unit to it.
  • the pre-cursor (coconut shells) will be impregnated with chemicals and will be used in the reactor for enhanced activation/functionalization through the chemical route, in addition to physical activation by steam.
  • coconut shells are loaded from the top and supported on a slide gate valve at the bottom.
  • the bed is ignited near the slide gate valve with limited supply of air (air flux rate between 80-100 g/m 2 s or oxidizer flux between 18-23 g/m 2 s) sucked into the reactor from the top with the help of a blower.
  • air air flux rate between 80-100 g/m 2 s or oxidizer flux between 18-23 g/m 2 s
  • a thin high temperature reaction zone is established upon ignition. This reaction zone generally propagates upwards after ignition leaving a hot char zone below it.
  • the reaction zone propagates upwards with a raw material consumption rate of 70-85 g/m 2 s.
  • superheated steam is supplied at a rate of 70-110 g/m 2 s into the char bed zone from the top of the reactor.
  • the steam is evenly distributed along the entire length of the hot-char bed with the help of a specially designed pipe with multiple injection ports.
  • a certain fraction of the total steam flow is injected into the oxidation zone to control the raw material consumption rate.
  • hot char reacts with steam and forms activated carbon.
  • the produced activated carbon is removed periodically from the bottom of the reactor using a slide gate valve; this procedure also ensures that the main reaction zone is fixed at a particular desirable location in the reactor and used to control the residence time.
  • the location of the reaction zone is inferred from the thermocouple measurements.
  • the producer gas from the reactor is cooled and cleaned with the help of a scrubber.
  • the producer gas is then burned at the exit using an exhaust gas burner.
  • the hot gas from the exhaust burner is used for superheated steam generation which is used for activation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Combustion & Propulsion (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne un procédé autonome à une seule étape d'activation in situ pour la synthèse de charbon actif à partir de résidus agro-chimiques. L'invention concerne la production de charbon actif (AC) en une seule étape par activation physique à l'aide de vapeur en tant qu'agent d'activation et biomasse ligno-cellulosique en tant que précurseur. Le charbon actif (AC) est produit dans un processus en continu dans un réacteur à lit fixe directement à partir de coques de noix de coco sans qu'il soit transformé en charbon de bois et sans utiliser de source de chaleur externe. Il s'agit d'un procédé autonome selon lequel l'énergie thermique requise pour le processus d'activation (réaction endothermique), est fournie par oxydation partielle de substances volatiles (réaction exothermique). De plus, l'énergie thermique requise pour la génération de vapeur est fournie par combustion du gaz producteur de produit, ce qui rend le procédé autonome.
PCT/IN2020/050732 2019-08-23 2020-08-21 Procédé autonome à une seule étape d'activation in situ pour la synthèse de charbon actif à partir de résidus agro-chimiques WO2021038583A1 (fr)

Applications Claiming Priority (2)

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IN201941034013 2019-08-23
IN201941034013 2019-08-23

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WO2021038583A1 true WO2021038583A1 (fr) 2021-03-04

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113830856A (zh) * 2021-10-09 2021-12-24 华北电力大学 一种协同沼液净化的飞灰连续活化装置及方法
CN117025242A (zh) * 2023-10-09 2023-11-10 江苏省环境工程技术有限公司 一种移动式秸秆炭化还田设备及方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
MINKOVA V ET AL.: "Effect of water vapour and biomass nature on the yield and quality of the pyrolysis products from biomass", FUEL PROCESSING TECHNOLOGY, vol. 70, 2001, pages 54 - 58, XP055796116, DOI: 10.1016/S0378-3820(00)00153-3 *
PARASKEVA P ET AL.: "Production of activated carbon from agricultural by-products", J CHEM TECHNOL BIOTECHNOL, vol. 83, 2008, pages 581 - 592, XP055796112, DOI: 10.1002/jctb.1847 *
SATYA SAI P M ET AL.: "Production of Activated Carbon from Coconut Shell Char in a Fluidized Bed Reactor", IND. ENG. CHEM. RES., vol. 36, 1997, pages 3625 - 3630, XP055796121, DOI: 10.1021/ie970190v *
YAHYA M A ET AL.: "Agricultural bio-waste materials as potential sustainable precursors used for activated carbon production: A review", RENEWABLE AND SUSTAINABLE ENERGY REVIEWS, vol. 46, 2015, pages 218 - 235, XP055796114, DOI: 10.1016/j.rser. 2015.02.05 1 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113830856A (zh) * 2021-10-09 2021-12-24 华北电力大学 一种协同沼液净化的飞灰连续活化装置及方法
CN117025242A (zh) * 2023-10-09 2023-11-10 江苏省环境工程技术有限公司 一种移动式秸秆炭化还田设备及方法
CN117025242B (zh) * 2023-10-09 2024-01-02 江苏省环境工程技术有限公司 一种移动式秸秆炭化还田设备及方法

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