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Study of the carbonization and activation of different lignocellulosic precursors for the elaboration of activated carbons with controlled porosity

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HAL Id: hal-02799598

https://hal.inrae.fr/hal-02799598

Submitted on 5 Jun 2020

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Study of the carbonization and activation of different lignocellulosic precursors for the elaboration of activated

carbons with controlled porosity

Martin Pajot, Benoît Cagnon, Stéphanie de Persis, Jean-Paul Charpentier, Marjorie Roulet, Alain Pineau, Sylvie Bonnamy

To cite this version:

Martin Pajot, Benoît Cagnon, Stéphanie de Persis, Jean-Paul Charpentier, Marjorie Roulet, et al..

Study of the carbonization and activation of different lignocellulosic precursors for the elaboration of activated carbons with controlled porosity. Exploring lignocellulosic biomass! Explorons la biomasse lignocellulosique !, Jun 2016, Reims, France. 2016. �hal-02799598�

(2)

Martin PAJOT 1,2 , Benoît CAGNON 1 , Stéphanie de PERSIS 2 , Jean-Paul CHARPENTIER 3 , Marjorie ROULET 1 , Alain PINEAU 1 , Sylvie BONNAMY 1

Study of the carbonization and activation of different lignocellulosic

precursors for the elaboration of activated carbons with controlled porosity

1

ICMN-Interfaces, Confinement, Matériaux et Nanostructures, CNRS, Orléans, France

2

ICARE-Institut de Combustion Aérothermique Réactivité et Environnement, CNRS, Orléans France

3

INRA-Institut National de la Recherche Agronomique, plateforme GénoBois, Orléans, France

Is it possible to produce activated carbons from tomato plants?

Context

Conclusion

Materials Energy

Activated Carbons Solid Fuels

Valorization of Lignocellulosic

Biomass

PYROLYSIS

gas, liquid

GASIFICATION

CO + H

2

COMBUSTION

Heat, CO

2

+ H

2

O

PHYSICAL ACTIVATION CHEMICAL ACTIVATION

 First tests of AC elaboration: very good result (without optimization) with tomato plants: textural properties fitted for water treatment

 activation optimization required to control porosity for a given application

Perspective: development of a predictive method to estimate the mass and the textural properties of the final AC

based on the study of the raw material: elementary analyses, biochemical composition, FTIR, XRD, Calorimetry, TGA curves, modelling For activated carbons => control of the porosity => for which application?

For solid fuels => High Heating Value (HHV), modelling of pyrolysis and secondary gas-phase reactions

Thermal behavior of Raw Material and lignocellulosic compounds

Miscanthus

Olive pomaces

Tomato

plants

OPTIMIZATION via the the study of the CARBONIZATION/PYROLYSIS COMPLEX for a lignocellulosic precursor due to:

-differences in reactivity between hemicellulose, cellulose and lignin -the competition of the reactions accompanying their decomposition

KNOWLEDGE OT THE RAW MATERIAL MANDATORY:

Poplar Wood

Carbonization Ar or N

2

500-800°C

Activation

H

2

O or CO

2

or O

2

up to 800°C

Activating Agent H

3

PO

4

or HNO

3

Carbonization Ar or N

2

500-800°C

Raw material from agricultural and agro-alimentary wastes

Elementary analysis, biochemical composition, FTIR, XRD, Thermal decompositions by thermogravimetry (TGA-DTA)

TGA-DTA carried out on all the lignocellulosic precursors and on the three compounds (H., C., L.) => estimation of their respective contribution in the final mass of the solid phase (chars and activated carbons)

Identification of the characteristic peaks

for lignocellulosic compounds Lignin decomposes over a wide

temperature range whereas hemicellulose and cellulose have characteristic peaks

Experimental conditions:

Tfinal: 800°C-1h Heating rate: 20°C.min-1

Vector gas: argon Flow: 160 mL.min-1

L. = 320°C C. = 350°C

H. = 250°C

Hemicellulose (H.) Cellulose (C.)

Lignin (L.)

Lignocellulosic compounds (commercial)

 Natural deconvolution of H. and C. for olive pomaces and miscanthus and L. is hidden.

 H. peak is less pronounced for tomato plants and poplar wood.

Thermal decomposition of the compounds inside the vegetal matrix

Thermal evolution followed by charring in an oven => Carbonization was done is several steps as a function of the previous thermograms

Grinding

Ball mill

+ H

3

PO

4

85%

Blending

Stirring 30 min

80°C

Drying

Under air 15 hours

110°C

Carbonization

Under Argon 500°C

40 min bearing

Rinsing/Filtering Product

obtained

HCl +

37%

Stirring 20 min

Filtering with distilled water until obtention of a neutral solution (pH = 7)

Raw material Activated

Carbon?

Drying

Stove 15 hours

50°C

Hemicellulose and chars Cellulose and chars Lignin and chars

Microporosity characterized by nitrogen adsorption at 77 K and comparison with a commercial AC

+ +

Carbonization of the pure compounds

 Different thermal behaviors as a function of the raw material.

The thermal decomposition of Lignin seems to be more complex than Hemicellulose and Cellulose.

 Optimization and modelling of the carbonization step required (whatever the activation method) as a function of the raw material in order to control final textural properties of the activated carbon.

 Analysis of the obtained data by means of a kinetic model required to better understand their

thermal decomposition

The isotherm shape indicates presence of

micropores and mesopores

Textural properties obtained from N

2

77K adsorption isotherm

Wo (cm3/g) Lo1 (Å) SBET (m²/g) Sext (m²/g) Sm icro (m²/g) Stotal (m²/g)

Tomatoe AC 0.38 22.1 1090 404 344 748

Commercial AC 0.39 12.7 1077 256 614 870

Very good result obtained without any optimization:

AC from tomato plants has textural properties closed to commercial AC used for water treatment

0 0.2 0.4 0.6 0.8 1 1.2 1.4

0 5 10 15 20 25 30 35 40 45 50

Differential pore volume (cm3/g)

pore width (angstrom)

AC from tomatoe plants Commercial AC

0 100 200 300 400 500 600

0 0.2 0.4 0.6 0.8 1 1.2

Volume adsorbé (cm3/g STP)

P/P0 AC from tomatoe plants

Commercial AC

Olive pomaces Miscanthus

Poplar wood Tomato plants

AC from tomato plants

 Commercial AC

P/P0

0 0.2 0.4 0.6 0.8 1.0

0

Adsorbed volume (cm3 /g STP )

100 200 300 400 500 600

Confirmation by the distribution size of micropores by DFT method

AC from tomato plants

 Commercial AC

Differential pore volume (cm3 /g )

Pore width (Angström)

Wo: specific microporous volume;

L01: mean microporous size; SBET: BET surface;

Sext: external surface;

Smicro: microporous surface Stotal: total surface

Références

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