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Proceedings Venice 2010, Third International Symposium on Energy from Biomass and WasteVenice, Italy; 8-11 November 2010

2010 by CISA, Environmental Sanitary Engineering Centre, Italy

SUPERCRITICAL WATER GASIFICATIONOF MODEL COMPOUNDS: INTERACTIONS

BETWEEN GLUCOSE AND GLYCEROL

Q. WU*, E. WEISS-HORTALA*, S. BULZA** AND R. BARNA*

* Université de Toulouse, Mines Albi CNRS, ALBI, France

** Universitatea Politehnica Timisoara, Romania

SUMMARY: Super Critical Water Gasification (SCWG: P>22.1 MPa, T>374°C) converts

organic compounds in species with high chemical energy (hydrogen, light hydrocarbons) with a

largely neutral CO2 balance. To observe interactions between two model molecules representing

the main organic byproducts: glucose and glycerol, batch experiments have been carried out with

5 mL autoclaves. The experiments have been performed in similar conditions with the pure

components and in mixture: 0.5 mol L-1

of organic matter and 0.025 to 0.1 mol L-1

of K2CO3 as

catalyst. The range temperature and pressure were 450-600°C and 20-28 MPa. The reaction time

varied from 15 to 240 min. H2, CO2, CH4 and C2H6 were the main gas products. The interaction

between glycerol and glucose in a mixed solution was very weak. A high temperature and the

use of K2CO3 allowed to improve the gasification efficiency and the hydrogen production. The

highest gasification efficiency of 70% and hydrogen yield of 1.5 mol/mol mixture was obtained

by using 0.1 mol L

-1

of catalyst at 600°C and 25 MPa.

1. INTRODUCTION

Wet biomass or comparable residues can be considered as renewable resources for sustainable

energy systems. Super Critical Water Gasification (SCWG: P>22.1 MPa, T>374°C) is a novel

way of treatment, where water acts as solvent and reactant (Clifford, 1993; Kruse and Dinjus,

2007). Supercritical water converts biomass into species with high chemical energy (hydrogen,

light hydrocarbons) with a largely neutral CO2 balance. The process is considered interesting for

biomass or organic residues with high water content (>30%). It allows the separation at high

pressure of H2 from the solution containing dissolved CO2, favouring sustainable solutions for itsuse/storage. SCWG process is under research, large scale industrial applications are not known

(Kruse, 2009).

Physico-chemichal properties of supercritical water are different from liquid water, implying

a high reactivity with organic compounds. The global reaction expected for glucose is as follow:

2226126 6126 CO H O H O H C +→+ (1)

However this reaction is not complete and some concurrent reactions could conduct to methane

and/or carbon monoxide production or lights hydrocarbons. Particularly, in presence of water,



Venice 2010, Third International Symposium on Energy from Biomass and Waste

carbon monoxide can react at high temperature and in presence of catalyst and produce hydrogen

and carbon dioxide (water gas shift reaction).

Biomass has a complex and variable composition of organic compounds and salts. The

particular properties of water in the region of its critical point lead (including salt precipitation)

to the quantitative hydrolysis and decomposition of biomass or organic residues in more simple

molecules which react forming different products distributed in gas, liquid or solid phases (Kruseand Dinjus, 2007). A large part of the experiments developed in laboratories replace

biomass/organic waste by model components. So glucose, hydrolysis product of cellulose, often

replaces cellulose/hemicelluloses (Matsumura et al., 2007) or syrupy residues. Glycerol is also

interesting because it is a sub product (residue) of the industrial process of biodiesel, which has

an important improve (Bühler et al., 2002). Moreover, glycerol composes also vinasses. In view

to model SCWG of syrupy residues, the interaction between glucose and glycerol should be

studied.

The literature shows that glucose gasification is efficient in batch and continuous process

(Holgate et al., 1995; Lee et al., 2002; Kruse and Gawlik, 2003; Yoshida et al., 2007; Weiss-

Hortala et al., 2010) in presence of catalyst. Watanabe et al. (2007) studied the conversion of

glycerol into acrolein and observed its low degradation for long reaction times in their operating

conditions (close to supercritical point). They showed that H2SO4 addition enhanced the

conversion efficiency into acrolein. A more complete study of reaction mechanisms showed that

a long reaction time disfavors acrolein production and favors gasification (Bühler et al., 2002).

Antal et al. (1999) were interested by the gasification process with carbon-based catalyst and

obtained a quasi-total conversion of glycerol. They noted the important catalytic effect of the

reactor surface. Other studies were carried out with Ru/Al2O3 catalyst (Byrd et al., 2008),

Na2CO3 catalyst (Xu et al., 2009) or Ru/ZrO2 catalyst (May et al., 2010); Ru-based catalysts are

efficient to convert glycerol and produce hydrogen in a short reaction time, while catalytic effect

is not significant. In the present study, the choice of catalyst is oriented towards alkaline instead

of metallic ones. Alkali salts are used to promote the water gas shift reaction (Sutton et al., 2001;Matsumura et al., 2005; Yanik et al., 2008) and to model inorganic compounds of a real biomass.

We have chosen an experimental SCWG approach in batch reactor to observe interactions

between the two model molecules representing in our experiment main organic components of

organic byproducts: glucose and glycerol.

2. EXPERIMENTAL STUDY

2.1 Reactor and reagents

The batch reaction was conducted in stainless steel 316 mini-autoclaves (V = 5 mL). The innerdiameter was 8.5 mm and the outer diameter was 31.4 mm. Two parts composed the mini-

autoclaves and a cupper joint was used in order to improve the watertight quality. The volume

being low, each experiment was carried out with 5 mini-autoclaves, running simultaneously.

The pressure was kept constant by adjusting the solution quantity as function of reaction

temperature. The mass of initial solution varied from 0.362 g (T=600°C) to 0.558 g (T=600°C).

The pressures varied from 20 to 28 MPa. The reaction, at the desired temperature, was conducted

by placing simultaneously 5 mini-autoclaves in the preheated muffle oven (Nabertherm

L5/11/P320). A heating time (about 10 min) is necessary to reach the desired temperature in the

system. After the reaction time, the autoclaves were cooled down in air jet to room temperature

(25 ± 2°C) during about 26 min.

Then the autoclaves were placed in the sampling system and the volume was scanned bynitrogen at atmospheric pressure. The overpressure obtained by opening the autoclave was




measured by a manometer. The volume of the system was 16.7 mL. The total mol number of the

gas recovered in the system by the mini autoclave openening was calculated (P, V and T known).

The gas was collected in a sampling bag under nitrogen flush. The liquid phase was collected

with a filtering syringe. The reactor was washed (by water) and the solid phase recovered by

filtration.

Glucose powder (C6H12O6, water free, Prolabo), glycerol solution (C3H8O3, 86-88%, Fluka)and ultra-pure water were used as raw materials to prepare the initial solutions. The solutions of

pure compounds, glucose or glycerol, were prepared at a concentration of 0.5 mol L-1

. The

mixture solutions were composed by 0.25 mol L-1

of glucose and 0.25 mol L-1

of glycerol.

K2CO3 (99.0-100.0%, Prolabo) was employed as catalyst, the molar ratio between organic

reactant and K2CO3 varies from 1:1 to 20:1.

2.2 Experimental procedure

The gas product was analyzed by a gas chromatograph (Agilent GC-3000 with 4 columns and 4

TCD detectors). The gases analysed are H2, CO2, CO, CH4, C2H6, C2H4 and C3H8. The gas phase

of each autoclave was analysed, but the results presented in this study are an average of the 5mini-autoclaves analyses.

A TOC analyser (Shimadzu TOC-5050) measured the total amount of carbon (organic and

inorganic) in the liquid phase after reaction.

2.3 Presentation of experimental datas

The main objective of the work is to determine the gasification efficiency of the process, i.e. the

conversion of initial organic matter from the liquid phase to the gas phase. The gasification

efficiency (GE) is defined as follow and expressed in percentage:

100×=

∑

reagent organicof massinitial

igasof mass

G i

E (2)

The second goal is to increase the part of hydrogen into the gas phase, particularly by promoting

the water gas shift reaction. So, the yield of each gas (Yi) is defined such as:

100×=

reagent organicof number molinitial

igasof number molY i (3)

3. RESULTS AND DISCUSSION

To study the interaction between glycerol and glucose, experiments were realized with pure

substances and with mixture of the two compounds. At first, the interaction was studied

comparing the gasification efficiency of pure component and mixture. Then, the influences of

temperature, catalyst on the gasification of mixture solution were investigated.

3.1 Study of interactions between glucose and glycerol

As it was mentioned previously, glucose and glycerol are obtained in different waste andparticularly vinasses. As regards to lignin or its model compounds (Yoshida and Matsumura,




2001; Weiss-Hortala et al., 2010), which influence glucose degradation, a similar method was

employed. Gas amounts of solutions containing separately glucose or glycerol, obtained under

the same operating conditions, were “theoretically” summed. This theoretical sum was compared

to the experimental value obtained for the mixture of the both molecules. If glucose and glycerol

interact during SCWG, the theoretical sum should be different from the experimental value.

In order to verify the possible effect of glycerol on the gasification of glucose, threeexperiments were conducted with a solution of glucose (0.54 mol L

-1), a solution of glycerol

(0.54 mol L-1

) and a solution containing glucose (0.54 mol L-1

) and glycerol (0.54 mol L-1

) at

525°C and 25 MPa. The comparison, illustrated in Figure 1, concerns the experimental amounts

of the main gas (CH4, CO2, H2, C2H6 and C2H4) and the total gas value. Theoretical value

represents the theoretical sum of gas production from glucose solution and glycerol solution.

Experimental value is the experimental gas amount obtained with the mixture solution. Previous

experiments using only glucose were realized with a concentration up to 1 M. In this range, the

glucose concentration was not a limitative factor of the gasification (proportionality between gas

produced and concentration), so the upper concentration of each compound employed in this

study was 0.54 mol L-1

.

Taking into account Equation 1, the total gasification of 1 mol of glucose conducts to 18 mol

of gas whose 12 mol of hydrogen. A similar equation written for glycerol (C3H8O3) conducts to 7

mol of hydrogen and 3 mol of carbon dioxide. The experiments presented on Figure 1 were

realized with 0.432 g of solution (= 0.23 mmol of each organic compound). The gas amount of

experiment conducted with glucose (4.1 mmol) should be higher than with glycerol (2.3 mmol),

but results in Figure 1 show that gasification is more efficient for glycerol than glucose. It could

be due to the higher polymerisation ability of glucose: Sinağ et al., (2004) explained this

behavior by favoring phenol formation and furfurals after a long reaction time (1 h). The gas

production from glucose is lower than that expected, indicating that the reaction is not complete.

For glucose, a ratio of about 2 mol of gas per mol of glucose is obtained being in accordance

with literature (Hao et al., 2003; Matsumura et al., 2005).

Figure 1. Comparison of gas production as function of kind of solutions under the same

operating conditions: glucose at 0.54 M; glycerol at 0.54 M; theoretical sum of the two

previous values; solution containing glucose and glycerol each at 0.54 M. T = 525°C,

P = 25 MPa, without catalyst and during 1 h.




The hydrogen quantity is lower than that of some published results, but operating conditions,

catalyst and process (batch or continuous) have a great influence on the process results. The

experiments presented were carried out without added catalyst. Hao et al. (2003) obtained also a

CO2 amount 3 times higher than H2.

For glycerol, the ratio is close to 3 mol of gas per mol or glycerol. This result is also in

accordance with the ratio obtained by Antal et al. (1999) in batch experiments with similaroperating conditions. Moreover, the molar ratios of hydrogen and carbon dioxide are also close

to those obtained by Antal et al. (1999). The part of methan is higher with glycerol than glucose

and it strongly depends from the catalyst (Sinağ et al., 2004).

The experimental value of gas production obtained with a mixture solution (1.02 mmol) is

close to the theoretical sum obtained with the pure compounds (0.97 mmol). This behavior

indicates that there are few interactions between glucose and glycerol molecules during the

gasification process. Concerning each gas produced: H2, CO2, CH4, the experimental values of

gas production are also close to the theoretical values.

At this stage, the modeling of SCWG of glucose and glycerol solutions seems to be a simple

sum of each pure component under the same operating conditions. However, literature indicates

that the effect of temperature has opposite effects on the gas production. In fact, experimental

datas of Byrd et al. (2008) and a thermodynamic analysis of Voll et al. (2009) indicates that an

increase of temperature conducts to:

a decrease of H2 and CO2 proportion and an increase of CH4 for glycerol solutions

an increase of H2 and CO proportion and a decrease of CH4 and CO2 for glucose solutions.

As regards theses informations, the gasification performance of a mixed glycerol / glucose

solution should be studied as function of different operating conditions. In this part of our

research, the effects of temperature and catalyst were investigated.

3.2 Influence of operating conditions

In this part, solutions were prepared with glucose and glycerol. The total concentration of organic

compound was 0.5 mol L-1

such as 0.25 mol L-1

of each pure compound. K2CO3 was used as

catalyst and the moles ratio between [mixture]/[catalyst] varies from 5:1 to 20:1 and the

temperature varies from 450 to 600°C.

3.2.1 Influence of temperature

Figure 2 shows the comparison of gasification efficiency (GE, Equation 2) as function of reaction

temperature.

Results are presented also with or without catalyst. At moderated temperature (450°C and

500°C) gasification efficiency is low (33% and 35%), but catalyst improves the conversion intogas (54% and 59%). At the highest temperature (600°C), the gasification efficiency is higher

(close to 70%) and the effect of catalyst is weak. According to the literature, an increase of the

temperature and the presence of an alkaline catalyst favor the gasification of organic compounds

(Kruse and Dinjus, 2007). Under the operating conditions, the total conversion is not reached for

the initial organic matter; we suppose that the catalytic effect of the reactor influences also the

reaction (Antal et al., 1999).

Figure 3 presents the variation of gas yield (Yi, Equation 3) as function of temperature for

solutions with and without catalyst. As shown in Figure 3 (a) and (b), carbon monoxide is not a

final product of the process. In conclusion, CO is not a main gas obtained during the gasification

process under the tested operating conditions.

Without catalyst (Figure 3 a) the yields of CH4 and CO2 increase significantly with thetemperature, those of H2 and C2H6 also increase while those of C2H4 and C3H8 stay constant.




Figure 2. Influence of temperature on gasification efficiency of glucose and glycerol solutions in

batch reactor (1 h). [glucose] = [glycerol] = 0.25 M, 25 MPa, [K2CO3] = 0.025 M.

As regards thermodynamic behavior of glucose and glycerol, an increase of temperature has

opposite effects on H2 and CH4 generation but should decrease the part of CO2. Results from

Figure 3 (a) do not confirm a decrease of carbon dioxide production. This difference could be

attributed to the rate of the competitive reactions and the role of catalysts (alkaline and reactor

inner surface). At 600°C, the gasification is more efficient but the hydrogen amount is

comparable to the value obtained with lower temperatures.

With catalyst (Figure 3 b) the yields of CH4 and CO2 increase almost linearly with the

temperature while H2 present a fluctuation. Results from Figure 3 (b) indicate also that combined

thermodynamic and kinetic can explain the increase of CO2 production. However, the profileobtained for hydrogen could be the result of the opposite thermodynamic behavior. Under the

operating conditions, it seems that thermodynamic of glucose degradation determine the

gasification profile between 500 and 550°C. This point should be developed in the future using

solutions at various concentrations of glucose and glycerol.

Maximum yield of CH4, CO2 and H2 are obtained for samples with and without catalyst at

600°C, which is in accordance with the maximum gasification efficiency.

a




Figure 3. Influence of temperature on gas yield of glucose and glycerol solutions in batch

reactor, without (a) or with (b) catalyst. T varies from 450-600°C, P = 25 MPa,

[glucose] = [glycerol] = 0.25 M, [K2CO3] = 0.025 M, time = 1 h.

Figure 4. Influence of temperature on gas fraction of various solutions treated by batch SCWG

process, during 1 h. (a): glycerol solution; (b): glucose solution; (c): theoretical sum of

a and b; (d): experimental value of a glucose and glycerol solution. [glucose] =

[glycerol] = 0.54 M, 25 MPa, [K2CO3] = 0.025 M.

(a)

(c)

b

(b)

d




In order to explain the previous results and study the possible interactions between glucose and

glycerol, gas composition (only CO2, H2 and CH4) as function of temperature was compared for

solutions of glucose and glycerol or either of them.

Figure 4 (a) and (b) shows the molar fraction of gas produced from glycerol solution and

glucose solution. For the glycerol solution (Figure 4 a), gas fraction of CO2 changes slightly from

45% to 43%, while H2 fraction decreases from 51 to 35%, with an important jump in the range of 500-550°C. The methan fraction increases quasi linearly. Only the increase of methan fraction is

in accordance with the thermodynamic model. Concerning H2 and CO2, a cumulative effect of

thermodynamics and kinetics may explain the profiles.

For glucose solution (Figure 4 b, only 3 experiments), gas fraction of CO2 drops linearly from

88% to 48% and that of H2 increasse linearly from 11% to 28%. The part of methan stays

constant. The decrease of CO2 fraction and the increase of H2 fraction in the gas phase is in

accordance with the thermodynamic prediction.

The results of glucose and glycerol solutions are combined to build a theoretical profile of the

gas fraction (Figure 4 c) and to be compared with the experimental dats (Figure 4 d). The graphs

present the same temperature dependence shapes and quasi the same fluctuations, even if the

number of points is different. The strong resemblance of CO2, H2 and CH4 repartition between

the theoretical values and the experimental values further proves that there are no major

interactions between glucose and glycerol during the gasification in supercritical water.

However, influences on H2 and CH4 gas fractions can be observed.

To conclude this part, the high gasification temperature enhances the gasification of glucose

and glycerol solution. The catalyst role is more efficient at lower temperatures (450-500°C) for

the gasification efficiency and the catalyst favors the generation of H2. The best gasification

efficiency and the highest yields of CH4, CO2 and H2 are obtained at 600°C for samples with

catalyst. Under the operating conditions, gasification of glucose and glycerol solutions seems to

be the combination of behaviors of each pure substance. Therefore, the influence of catalyst

concentration on gasification will be studied at 600°C.

3.2.2 Influence of catalyst concentration

Figure 5 illustrates the influence of catalyst concentration on gasification efficiency (a) and gas

yield (b) for mixture solutions at 600°C. The molar ratio between K2CO3 (catalyst) and mixture

varies from 0 to 1:5.

Figure 5 (a) shows that gasification efficiency rises slightly from 62% to about 69% at 600°C

(maximum at a ratio of 1:20). No real influence on gasification efficiency can be observerd by

increase of the catalyst ratio beyond 1:20. The molar proportion of catalyst compared to amount

of organic compounds is not a limitative factor of the gasification efficiency. This observation

indicates that the catalyst does not play an important role directly on the substrate at this

temperature. K2CO3 is a catalyst of the water gas shift reaction, meaning that the reaction

between CO and H2O is favored.

The variation of gas composition is presented on Figure 5 (b). The yield of H2 increases

significantly from 0.54 to 0.86 mol/mol mixture while the yields of CO2, CH4 and C2H6 keep

stable with the increase of the catalyst concentration. The fluctuation of H2 proportion obtained

at a ratio of 1:10 seems to be linked to the slight decrease of the gasification efficiency. Only a

complete study of other ratio arond this value could confirm the presence of this decrease.

However, the general profile indicates that K2CO3 plays an important role to improve the H2

production. The total organic carbon content (TOC) of the solutions confirms that the TOC

removal increases as function of catalyst concentration increase (not shown).

According to the previous results, K2CO3 favors slightly the gasification at 600°C, and theincrease of its concentration improves the generation of H2.




Figure 5. Influence of catalyst concentration on gasification efficiency (a) and gas yield (b) of

glucose and glycerol solutions during 1 h of batch SCWG process. [glucose] =

[glycerol] = 0.25 M, 25 MPa, T = 600°C.

4. CONCLUSIONS

Glucose and glycerol, model molecules of parts of biomass, have been widely studied in SCWG

process, but not the interaction between those two substances. The aim of the work was to

investigate the supercritical water gasification of mixed glucose and glycerol solution in a batch

reactor. With a concentration of organic substances at 0.5 mol L-1

and K2CO3 used as catalyst,

the influences of gasification temperature (450-600°C) and catalyst concentration (K2CO3) have

been studied. The main conclusions are:

the interaction between glycerol and glucose during SCWG of an equimolar in a mixed

solution is very weak. A mixed solution produces more gas than solution of pure substances,

close to the theoretical prediction.

high temperature (600°C) enhances the gasification of mixed glucose and glycerol solutioncompared to relatively lower temperatures (450-500°C).

(a)

b




catalyst (K2CO3) improves hardly the gasification efficiency at 450 and 500°C but the effect

is less important at 600°C: it favors H2 generation.

In the future researches, the influence of concentration of mixed solution, reaction time and

pressure will be investigated.

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super critical water gasification glucose

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