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CL 640 : Research Methodology Term Project – I A Presentation On Pursuing efficient system of glucose transformation to levulinic acid: Homogeneous vs. heterogeneous catalysts and the effect of their co-action . Under the supervision of Prof . Ramgopal Uppaluri Indian Institute of Technology Guwahati Guwahati-781039,India.

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 Catalytic conversion of glucose to LA in the presence of both homogenous and heterogeneous co-catalyst system have so far not been investigated in detail.  A homogeneous catalyst having only a bronsted acid site is insufficient to produce an acceptable amount of LA.  Presence of Lewis site is inevitable for a reasonable yield of LA .  Use of only homogeneous catalyst system in synthesis of LA suffers from difficulties in product separation and product recovery ..

Parameters and Critical Parameters. Parameters  Volume of the reactor (50 mL)  Initial amount of the glucose (180 mg)  Concentration of the dissolved metal chloride ( 5 mmol ).

Variables(IV, CIV, DV, CDV). Independent Variables (IV)  Reaction Time (15-180 min).

Functionalization. ACS. Activated Carbon. - - - - - -.

Methodology (Style of Experiment). 155 Glucose ACS Metal Chloride Set-I Glucose ACS-B Metal Chloride Set-ill 0.625 175 Varying Temperature HT Reactor 195 Varying Catalyst Load Glucose AC-PTSA Metal Chloride Set-II 15 30 60 120 180 1.25 2.5 5.

Interesting Observation. CaCl 2 f unctionalize activate carbon reduces the yield while same CaCl 2 use as homogenous catalyst, LA yield increases significantly..

Logical Statements. GLU Conversion • LA yield HMF yield NaCl caC12 MgC12 BaC12 znC12.

Logical Statements. —GLU Conversion —.—LA yield 100 80 60 40 20 30 60 90 120 150 180 Time, min.

Hypothesis (Without strong experimental validity).

H ypothesis (Without strong experimental validity).

13. 1 Best data observed in terms of LA yield is 61% Glucose conversion is found to be 100% 2 Reaction time to ↑ the yield is 2h . Optimum operating temperature is 175℃ 3 MIBK / H 2 O ratio is 2.33.

Subjective Inferences. 1 2.  Presence of both catalyst PTSA and CaCl 2 results remarkable yield of LA..

IIT Guwahati Wikipedia. Generalized Approaches to alter P/CP, IV/CIV, DV/CDV.

Improving Research Methodology. IIT Guwahati Wikipedia.

Feedstock Catalyst LA Yield Critical Findings 10 wt% Glucose Amberlyst 70 30-55 C% Yield is low due to absence of bronsted site in the catalyst. 50 g/L Glucose 0.05 g/L ZrPO 4 29 wt% - 0.1 M Glucose 1M H 2 SO 4 94 mol% Difficulties in separation due to homogeneous nature of catalyst. 20 g/L Glucose 20 g/L Fe/HY 62.0 mol% Formation of Humins is major problem. 0.35 M Glucose 7.2 M HCl 35 mol% Yield is low due to absence of lewis site in the catalyst, difficulties in separation. 2% Cellulose 0.02M CrCl 3 67 mol% Contains both lewis and bronsted site but homogenous in nature. 2% Cellulose 2% ZrO 2 53.9 mol% Effect of catalyst on i somerization of glucose to fructose is negligible. 5% Fructose 1.5 g/L InCl 3 45 mol% Contains both lewis and bronsted site but homogenous in nature.

Similar Research at IITG. Feasibility Available conversion Techniques : Hydrothermal liquefaction, Pyrolysis, Microwave. Feedstock In place of glucose unexplored lignocellulosic biomass contain higher amount of cellulose can be used as feedstock. Product Identification tools Analytical facilities at IITG : FTIR, HPLC, NMR etc..

Novelty Statement.  Co-catalyst system having lewis site and bronsted site are efficiently utilised for the production of LA from glucose monomer .  A novel PTSA immobilized activated carbon is used as bimetallic heterogeneous catalyst.  Introduction of h alf homogeneous and half heterogeneous catalyst system : AC-PTSA and CaCl 2 has remarkable effect on LA Yield..

Critical content analysis (Figures). PTSA and CaCl 2 supported activated carbon :.

Critical content analysis (Figures). Homogeneous Vs heterogeneous catalysis Vs LA yield :.

Critical content analysis (Figures). GLU Conversion LA yield HMF yield 80 60 40 20 Acs.g AC-PTSA *AC-PTSA.

Critical content analysis (Tables). Temperature GLU conversion LA yield(%) HMF yield(%) 155 82 05 30 175 90 58 02 195 95 40 02.

Catalyst loading GLU conversion (%) LA yield(%) HMF yield(%) 0.625 94 40 20 1.250 95 48 20 2.500 95 50 15 5.000 95 54 05.

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