This method describes the continuous production of methyl pentenone (MPO) in high yield using a fixed bed reactor equipped with multiple sidewall injection ports. The process involves reacting an excess of methyl ethyl ketone (MEK) with acetaldehyde in the presence of a cation exchange resin catalyst while acetaldehyde is introduced through the sidewall injection ports of the reactor. This technique enhances the yield of MPO and also reduces the complete consumption of the catalyst during the reaction
- Yield of MPO obtained is nearly 70% with a semi-batch addition of acetaldehyde in a mixed pool of MEK and sulfuric acid
- Cation exchange resin (e.g. Amberlyst-15), a heterogeneous catalyst, has advantages over sulfuric acid and prevents issues related to corrosion, salt handing and safety
- Fixed bed reactor (FBR) demonstrated for production of MPO in continuous mode.
- MPO yield increases from 55% to 85% by minimising acetaldehyde concentration from 1:2 to 1:18 (AcH: MEK) in the feed molar ratio in the reactor
- Low production cost and no effluent generation
- Steady state MPO yield obtained was nearly 80% (based on AcH) for 600 hours indicating the successful scale-up of the lab work to the pilot scale
- Catalyst life increased by two means due to side injection of acetaldehyde
- Costs of neutralization after each batch, salt handling and disposal were eliminated
- Avoids the need to handle hazardous sulfuric acid and eliminates the requirement for large amounts of water generally required in the conventional process
Based on an extensive study of reactor design and rate kinetics, a fixed bed reactor (FBR) has been demonstrated for the continuous production of methyl pentenone (MPO). The feed molar ratio of acetaldehyde (AcH) to methyl ethyl ketone (MEK) (ranging from 1:2 to 1:18) significantly impacts the MPO yield, which varies from 55% to 85%. Other parameters such as residence time (5-16 gm.min/ml) and temperature (343-363 K) have less pronounced effects. The data indicates that the MPO yield increases from 55% to 85% by minimizing the acetaldehyde concentration from a 1:2 to a 1:18 AcH:MEK feed molar ratio, consistent with rate kinetics observations. Pilot-scale experiments were conducted on an FBR with 5-6 side injections. Pilot-level experiments were performed at a scale-up volume ratio of 1:120, achieving a steady-state MPO yield of nearly 80% (based on AcH) for 600 hours, indicating the successful scale-up from lab work to pilot scale.
The invention is currently at the stage of Early Prototype development and/or validation in relevant environment.
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This technology provides important benefits in safety and environmental sustainability. Companies around the world are eager to adopt safer and greener processes and are willing to pay more for such innovations. This technology meets these needs, offering a safer and more environmentally friendly alternative conventional MPO manufacturing, which has a history of industrial accidents. This helps companies improve their reputation and move towards more sustainable practices.
Flavors & Fragnance industry
MPO is a crucial intermediate chemical for the production of Iso E Super. For both Iso E Super as well as MPO no alternatives are available. ISO E Super is a cornerstone product for the F&F Industry globally There are about 5 to 6 plants globally using the conventional process of manufacture of MPO. A typical plant capacity ranges from 1000 to 6000 TPA. The current invention has a potential to eliminate several expensive operations of conventional MPO processing like purchase of Sulfuric Acid catalyst and consumption of Caustic for neutralization, landfill cost for disposal of sodium sulfate
202021041062
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