ConfidentialA European Project supported within the Seventh Framework Programme for Research and Technological Development

Effective FeMo catalyst for the direct synthesis of dimethyl-and diethyl acetalsEuroBioRef Summer School

Castro Marina, Lecce, Italy, September 18th – 24th 2011Co-authors: Guillaume Tesquet (UCCS), Louise Jalowiecki-Duhamel (UCCS), Franck Dumeignil (UCCS)Jean-Luc Dubois (ARKEMA), Jean-Luc Couturier (ARKEMA), Mickaël Capron (UCCS) Speaker: Kaew-arpha Thavornprasert (CNRS-UCCS USTL)

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Choice of catalysts FeMo catalyst characterisation

“MoO3-Fe(MoO4)3 (or FeMo)[3,4] ” prepared by co-precipitation of (NH4)6MoO24.4H2O andFeCl3.6H2O, Tcalcination = 723 K, 2 h under air flow[5]

catalytic performance in comparison with- Mo12V3W1.2Cu1.2Sb0.5Ox

[1]

- 7% Re/TiO2

previously exhibiting interesting performances[2]

Fe2(MoO4)3,MoO3, andβ-Fe2(MoO4)3

crystalline phases

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" Drastic change in DMM selectivity under rich MeOH condition for FeMo catalyst giving the best obtainable DMM productivity of 4.6 kg.h-1.kgcat

-1 at 553 K with 56% conversion and very high selectivity of 90% "

Catalytic performance at 553 K

Comparison of catalytic activities in terms of DMM productivity

Catalytic test conditions Catalyst: 150 mg (diluted with 150 mg SiC)Activation: 623 K (1 h) in O2 flow for Mo12V3W1.2Cu1.2Sb0.5Ox

and Re/TiO2, no pretreatment for FeMoFeed compositions: MeOH/O2/He = 7.5/8.5/84 mol% (Poor Feed)

MeOH/O2/He = 40/13/47 mol% (Rich Feed)GHSV: 22 NL.h-1.gcat

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Results

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Gas Phase Dimethoxymethane (DMM) Production from Methanol:

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" Remarkable DEE productivity(1.04 kg.h-1.kgcat

-1) at 526 K with 31% conversion and 47% selectivity

over FeMo catalyst "MoO3-Fe2(MoO4)3

Catalytic performances evaluated at different Treaction

Gas Phase Diethoxyethane (DEE) Production from Ethanol:

Catalytic test conditions Catalyst: 150 mg (diluted with 600 mg SiC)Activation: 10 K.min-1 → 613 K (15 h) in O2/He flow (20/80),

Ftotal = 60 mL.min-1

Feed composition: EtOH/O2/He = 30.8/7/62.2 vol%GHSV: 26 NL.h-1.gcat

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Results

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Acknowledgement

The research led in this project has received funding from the European Union Seventh Framework Programme [FP7/2007 2013]

under grant agreement n°241718.

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