WO2013073977A1 - Method for production of nanoporous activated carbons with high nitrogen contents - Google Patents

Method for production of nanoporous activated carbons with high nitrogen contents Download PDF

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Publication number
WO2013073977A1
WO2013073977A1 PCT/PL2012/000123 PL2012000123W WO2013073977A1 WO 2013073977 A1 WO2013073977 A1 WO 2013073977A1 PL 2012000123 W PL2012000123 W PL 2012000123W WO 2013073977 A1 WO2013073977 A1 WO 2013073977A1
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WO
WIPO (PCT)
Prior art keywords
heating
depolymerisation
carbon
protonisation
activated carbons
Prior art date
Application number
PCT/PL2012/000123
Other languages
French (fr)
Inventor
Anna KUCIŃSKA
Jerzy ŁUKASZEWICZ
Original Assignee
Uniwersytet Mikołaja Kopernika
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Publication date
Application filed by Uniwersytet Mikołaja Kopernika filed Critical Uniwersytet Mikołaja Kopernika
Publication of WO2013073977A1 publication Critical patent/WO2013073977A1/en

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    • 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

Definitions

  • the invention is related to a method for production of nanoporous activated carbons with high nitrogen contents, in which chitosan is a basic raw material.
  • Activated carbons are versatile adsorbents used in many areas of technology and everyday life. Their adsorption properties result from a large surface area, developed microporous structure and high degree of reactivity connected with the occurrence of so- called superficial functional groups containing heteroelements - mainly oxygen, nitrogen and sulfur - on the surface of the carbons. This is why they are used for purification, decolourisation, waste disposal, dechlorination, separation and concentration, filtration, removal or modification of hazardous components of gases and liquids. Adsorption on activated carbon is of importance in many economical sectors and pertains to various areas, such as the food, pharmaceutical, chemical, petroleum and automotive industries, nuclear and vacuum technologies, as well as potable water purification, industrial and municipal waste treatment and industrial waste gases.
  • a method for carbon nitrogen enrichment which consists in obtaining activated carbon from lignin-cellulose raw material using phosphorous acid, washing out the impurities with water in a Soxhlet extractor, then impregnating with urea and heating under nitrogen.
  • the essence of the solution according to the invention is a method for production of nanoporous activated carbons with high nitrogen contents, characterised in that chitosan is swelled, next it is subjected to protonisation and depolymerisation, then it is mixed with a solution of carbonates and heated in an atmosphere with low chemical reactivity. Afterwards, it is treated with acid, washed out, filtered off and dried. For the washing and swelling, distilled water is used. Protonisation and depolymerisation are carried out using aqueous solution of HC1. After the protonisation and depolymerisation process, an aqueous solution of sodium carbonate is added. The heating is carried out under nitrogen at 600- 800°C for at least 1 hour. After heating, HC1 or HN0 3 is used.
  • the method enables one to obtain carbon materials with a de ⁇ veloped surface area and, at the same time, with high nitrogen contents, utilising commonly available chitosan - renewable bio- polymer - as a raw material for carbonisation.
  • the proposed method allows for manufacturing activated carbons with favourable properties, owing to the application of a novel procedure and cheap chemicals .
  • Example 1 First, to raw powdered chitosan (10 g) in a beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1M HC1, is added in order to protonise and depolymerise hydrophiiic groups. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na 2 CC>3 (20 cmx3x) at a concentration of 16.9% is added.
  • a strong acid solution 3 cmx3x
  • 1M HC1 1M HC1
  • the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20-800°C in a controlled atmosphere with a non-oxidising character and low chemical reactivity.
  • the heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C.
  • the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time.
  • the carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1M HCl, in a ratio of 6 cmx3x of acid solution per 1 g of carbon.
  • Example 2 First, to raw powdered chitosan (10 g) in a beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1M HCl, is added in order to protonise hydrophiiic groups and depolymerise. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na 2 C0 3 (20 cmx3x) at a concentration of 16.9% is added.
  • a strong acid solution 3 cmx3x
  • 1M HCl e.g. 1M HCl
  • the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20-800°C in a controlled atmosphere with a non-oxidising char ⁇ acter and low chemical reactivity.
  • the heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C.
  • the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time.
  • the carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1M HNO 3 , in a ratio of 6 cmx3x of acid solution per 1 g of carbon.
  • Example 3 First, to raw powdered chitosan (10 g) in a . beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1M HC1, is added in order to depolymerise and protonise hydrophilic groups. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na 2 C0 3 (20 cmx3x) at a concentration of 33.4% is added.
  • a strong acid solution 3 cmx3x
  • 1M HC1 1M HC1
  • the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20-800°C in a controlled atmosphere with a non-oxidising character and low chemical reactivity.
  • the heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C.
  • the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time.
  • the carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1 HC1, in a ratio of 6 cmx3x of acid solution per 1 g of carbon.
  • the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20- 800°C in a controlled atmosphere with a non-oxidising character and low chemical reactivity.
  • the heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C.
  • the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time.
  • the carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1M HC1, in a ratio of 6 cmx3x of acid solution per 1 g of carbon.

Abstract

Method for production of nanoporous activated carbons with high nitrogen contents, characterised in that chitosan is swelled, next it is subjected to protonisation and depolymerisation, then it is mixed with a solution of carbonates and heated in an atmosphere with low chemical reactivity. Afterwards, it is treated with acid, washed out, filtered off and dried. For the swelling, distilled water is used. Depolymerisation and protonisation are carried out using an aqueous solution of HC1. After the depolymerisation process, an aqueous solution of sodium carbonate is added. The heating is carried out under nitrogen at 600-800°C for at least 1 hour. After heating, HC1 or HNO3 is used.

Description

Methodi for production of nanoporous activated carbons with high nitrogen contents
The invention is related to a method for production of nanoporous activated carbons with high nitrogen contents, in which chitosan is a basic raw material.
Activated carbons are versatile adsorbents used in many areas of technology and everyday life. Their adsorption properties result from a large surface area, developed microporous structure and high degree of reactivity connected with the occurrence of so- called superficial functional groups containing heteroelements - mainly oxygen, nitrogen and sulfur - on the surface of the carbons. This is why they are used for purification, decolourisation, waste disposal, dechlorination, separation and concentration, filtration, removal or modification of hazardous components of gases and liquids. Adsorption on activated carbon is of importance in many economical sectors and pertains to various areas, such as the food, pharmaceutical, chemical, petroleum and automotive industries, nuclear and vacuum technologies, as well as potable water purification, industrial and municipal waste treatment and industrial waste gases.
A method for carbon nitrogen enrichment is known, which consists in obtaining activated carbon from lignin-cellulose raw material using phosphorous acid, washing out the impurities with water in a Soxhlet extractor, then impregnating with urea and heating under nitrogen.
The essence of the solution according to the invention is a method for production of nanoporous activated carbons with high nitrogen contents, characterised in that chitosan is swelled, next it is subjected to protonisation and depolymerisation, then it is mixed with a solution of carbonates and heated in an atmosphere with low chemical reactivity. Afterwards, it is treated with acid, washed out, filtered off and dried. For the washing and swelling, distilled water is used. Protonisation and depolymerisation are carried out using aqueous solution of HC1. After the protonisation and depolymerisation process, an aqueous solution of sodium carbonate is added. The heating is carried out under nitrogen at 600- 800°C for at least 1 hour. After heating, HC1 or HN03 is used.
The method enables one to obtain carbon materials with a de¬ veloped surface area and, at the same time, with high nitrogen contents, utilising commonly available chitosan - renewable bio- polymer - as a raw material for carbonisation. The proposed method allows for manufacturing activated carbons with favourable properties, owing to the application of a novel procedure and cheap chemicals .
Example 1. First, to raw powdered chitosan (10 g) in a beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1M HC1, is added in order to protonise and depolymerise hydrophiiic groups. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na2CC>3 (20 cmx3x) at a concentration of 16.9% is added. After scrupulous mixing, the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20-800°C in a controlled atmosphere with a non-oxidising character and low chemical reactivity. The heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C. After the intended temperature is reached, the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time. The carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1M HCl, in a ratio of 6 cmx3x of acid solution per 1 g of carbon. After adding the acid, a violent reaction occurs with liberation of gaseous C02.. Then, carbon is filtered off on a Biichner funnel, being washed with distilled water until pH = 7 (neutral) is reached. Next, in order to evaporate excess water, the prepared carbon is dried at 50°C. The obtained carbon is characterised by a significant surface area of 440 m2/g, high total volume of pores and high mass contents of nitrogen at 5.26%. The surface area of the carbonised chitosan containing microdomains in the form of Nax2xCOx3x crystallites (the sample before the final etching in 1M HCl) was distinctly smaller and amounted to 1 m2/g.
Example 2. First, to raw powdered chitosan (10 g) in a beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1M HCl, is added in order to protonise hydrophiiic groups and depolymerise. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na2C03 (20 cmx3x) at a concentration of 16.9% is added. After scrupulous mixing, the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20-800°C in a controlled atmosphere with a non-oxidising char¬ acter and low chemical reactivity. The heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C. After the intended^ temperature is reached, the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time. The carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1M HNO3, in a ratio of 6 cmx3x of acid solution per 1 g of carbon. After adding the acid, a violent reaction occurs with liberation of gaseous C02. Then, carbon is filtered off on a Buchner funnel, being washed with distilled water until pH = 7 (neutral) is reached. Next, in order to evaporate excess water, the prepared carbon is dried at 50°C. The obtained carbon is characterised by a significant surface area of 212 m2/g, high total volume of pores and high mass contents of nitrogen at 6.55%. The surface area of the carbonised chitosan containing microdomains in the form of Nax2xCOx3x crystallites (the sample before the final etching in 1M HN03) was distinctly smaller and amounted to 1 m2/g.
Example 3. First, to raw powdered chitosan (10 g) in a. beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1M HC1, is added in order to depolymerise and protonise hydrophilic groups. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na2C03 (20 cmx3x) at a concentration of 33.4% is added. After scrupulous mixing, the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20-800°C in a controlled atmosphere with a non-oxidising character and low chemical reactivity. The heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C. After the intended temperature is reached,' the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time. The carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1 HC1, in a ratio of 6 cmx3x of acid solution per 1 g of carbon. After adding the acid, a violent reaction occurs with liberation of gaseous C02. Then, carbon is filtered off on a Buchner funnel, being washed with distilled water until pH = 7 (neutral) is reached. Next, in order to evaporate excess water, the prepared carbon is dried at 50°C. The obtained carbon is characterised by a significant surface area of 106 m2/g, high total volume of pores and high mass contents of nitrogen at 6.08%. The surface area of the carbonised chitosan containing microdomains in the form of Nax2xCOx3x crystallites (the sample before the final etching in 1M HC1) was distinctly smaller and amounted to 1 m2/g. Example 4. First, to raw powdered chitosan (10 g) in a beaker, distilled water (5 cmx3x) is added. Then, a strong acid solution (3 cmx3x) , e.g. 1 HC1, is added in order to depolymerise and protonise hydrophilic groups. After scrupulous mixing, formation of the spongy chitosan mass swelled as a consequence of water absorption is observed. Next, an aqueous solution of sodium carbonate Na2C03 (20 cmx3x) at a concentration of 7.8% is added. After scrupulous mixing, the so-prepared mass is placed inside a heating unit ensuring controlled heating in the temperature range of 20- 800°C in a controlled atmosphere with a non-oxidising character and low chemical reactivity. The heating rate is 10°C/min up to the defined carbonisation temperature, i.e. 600°C. After the intended temperature is reached, the obtained carbon remains in the heating unit for 1 hour, and then until it's cooled to 50°C, remaining under constant nitrogen flow for the whole time. The carbon material obtained after carbonisation is treated with an aqueous solution of a strong acid, i.e. 1M HC1, in a ratio of 6 cmx3x of acid solution per 1 g of carbon. After adding the acid, a violent reaction occurs with liberation of gaseous C02. Then, carbon is filtered off on a Buchner funnel, being washed with distilled water until pH = 7 (neutral) is reached. Next, in order to evaporate excess water, the prepared carbon is dried at 50°C. The obtained carbon is characterised by a surface area of 19 m2/g, high total volume of pores and high mass contents of nitrogen at 7.34%. The surface area of the carbonised chitosan containing microdo- mains in the form of Nax2xCOx3x crystallites (the sample before the final etching in 1M HC1) was distinctly smaller and amounted to 1 m2/g.

Claims

Claims
1. Method for production of nanoporous activated carbons with high nitrogen contents, characterised in that chitosan is swelled, next it is subjected to protonisation and depolymerisation, then it is mixed with a solution of carbonates and heated in an atmosphere with low chemical reactivity. Afterwards, it is treated with acid, washed out, filtered off and dried.
2. Method according to claim 1, characterised in that distilled water is used for swelling.
3. Method according to claim 1, characterised in that protonisation and depolymerisation are carried out using an aqueous HC1 solution .
4. Method according to claim 1, characterised in that after protonisation and depolymerisation, an aqueous solution of sodium carbonate is added.
5. Method according to claim 1, characterised in that heating is carried out under nitrogen at 600-800°C for at least 1 hour.
6. Method according to claim 1, characterised in that after heating, HCl is used.
7. Method according to claim 1, characterised in that after heating, HN03 is used.
PCT/PL2012/000123 2011-11-14 2012-11-14 Method for production of nanoporous activated carbons with high nitrogen contents WO2013073977A1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016163899A1 (en) * 2015-04-09 2016-10-13 Nicolaus Copernicus University In Torun Activated carbons with a high nitrogen content and a high electric conduction and the method of manufacturing activated carbons, in particular the method of manufacturing electrodes

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Publication number Priority date Publication date Assignee Title
PL233944B1 (en) * 2018-12-20 2019-12-31 Instytut Agrofizyki Im Bohdana Dobrzanskiego Polskiej Akademii Nauk Method for obtaining bio-coal with high nitrogen content and the bio-coal obtained with this method

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JPH09155186A (en) * 1995-12-05 1997-06-17 Agency Of Ind Science & Technol Adsorbent
JP2003313021A (en) * 2002-04-19 2003-11-06 National Institute Of Advanced Industrial & Technology Metal-containing porous body and method for manufacturing the same
DE10313267A1 (en) * 2003-03-24 2003-11-20 Manfred Lottermoser Water filter e.g. for production of drinking water consists wholly or partly of chitin especially obtained from crab waste in food processing
US20050252373A1 (en) * 2004-05-11 2005-11-17 Shiflett Mark B Storage materials for hydrogen and other small molecules
JP2006225231A (en) * 2005-02-21 2006-08-31 Univ Of Miyazaki Activated carbon from chitinous matter as raw material and its manufacturing method
JP2008194600A (en) * 2007-02-13 2008-08-28 Miyazaki Tlo:Kk Adsorbent material made up of active carbon with high specific surface area using waste as raw material
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JPH09155186A (en) * 1995-12-05 1997-06-17 Agency Of Ind Science & Technol Adsorbent
JP2003313021A (en) * 2002-04-19 2003-11-06 National Institute Of Advanced Industrial & Technology Metal-containing porous body and method for manufacturing the same
DE10313267A1 (en) * 2003-03-24 2003-11-20 Manfred Lottermoser Water filter e.g. for production of drinking water consists wholly or partly of chitin especially obtained from crab waste in food processing
US20050252373A1 (en) * 2004-05-11 2005-11-17 Shiflett Mark B Storage materials for hydrogen and other small molecules
JP2006225231A (en) * 2005-02-21 2006-08-31 Univ Of Miyazaki Activated carbon from chitinous matter as raw material and its manufacturing method
JP2008194600A (en) * 2007-02-13 2008-08-28 Miyazaki Tlo:Kk Adsorbent material made up of active carbon with high specific surface area using waste as raw material
CN101780955A (en) * 2010-03-22 2010-07-21 哈尔滨工业大学 Chitosan activated carbon and preparation method thereof

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DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; 2 September 2010 (2010-09-02), LI, BAOQIANG ET AL: "Chitosan activated carbon and its preparation by metal ion activation and microwave carbonization", XP002692939, retrieved from STN Database accession no. 153:290503 *

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016163899A1 (en) * 2015-04-09 2016-10-13 Nicolaus Copernicus University In Torun Activated carbons with a high nitrogen content and a high electric conduction and the method of manufacturing activated carbons, in particular the method of manufacturing electrodes

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