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Continuous production of methylpentenone using cation exchange resin in fixed bed reactor

A technology of methyl pentenone and reactor, applied in the direction of cation exchange, ion exchange, ion exchange column/bed method, etc.

Pending Publication Date: 2022-03-29
INDIAN INSTITUTE OF TECHNOLOGY BOMBAY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a result, waste disposal costs account for a significant portion of production costs

Method used

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  • Continuous production of methylpentenone using cation exchange resin in fixed bed reactor
  • Continuous production of methylpentenone using cation exchange resin in fixed bed reactor
  • Continuous production of methylpentenone using cation exchange resin in fixed bed reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0093] A stainless steel fixed bed reactor SS-316 (length 470 cm, inner diameter 5.08 cm) was used for the reaction. The reactor was charged with catalyst Amberlyst-15 (3.15 kg). MEK was fed into the reactor using a pump at a rate of 8.67 gm / min in the main line. Such as figure 2 Acetaldehyde was fed to the column through 6 side injection ports at 0.9 gm / min (MEK 55.56% (w / w)) as indicated. Experiments were carried out at 363-368K and 5 barg with a total feed ratio of 1:3 (AcH:MEK) with a total feed flow rate of 18 kg / day to 18.5 kg / day (295 min residence time). The reactor is heated using electrical coils wrapped around the reactor column. The experiment was carried out continuously for 300 hours. It was found that the MPO yield varied from 75% to 80% (based on acetaldehyde) within 300 hours at an average feed molar ratio close to 1:3 (AcH:MEK). The MPO yield was verified by distillation. This result is very important because it demonstrates the broad application of Am...

Embodiment 2

[0096] A stainless steel fixed bed reactor SS-316 (length 470 cm, inner diameter 5.08 cm) was used for the reaction. The reactor was charged with catalyst Amberlyst-15 (3.15 kg). MEK was fed into the reactor using a pump at a rate of 8.67 gm / min in the main line. Such as figure 2 Acetaldehyde was fed into the column at 0.71 gm / min (MEK 55.56% (w / w)) through 6 side injection ports as indicated. Experiments were carried out at 363-368K and 5 barg with a total feed ratio of 1:3.5 (AcH:MEK) with a total feed flow rate of 18 kg / day to 18.5 kg / day (345 min residence time). The reactor is heated using electrical coils wrapped around the reactor column. The experiment was carried out continuously for 300 hours. MPO yields were found to vary in the range of 80% to 85% (based on acetaldehyde). The MPO yield was verified by actual distillation. This result is very important because it demonstrates the broad application of Amberlyst-15 in the production of methylpentenone on an ind...

Embodiment 4A

[0109] Example 4A: The experiment was carried out in a SS-316 batch reactor at 343K for 6 hours using 100 g of pure methyl ethyl ketone (MEK) and 10 g of Amberlyst-15. The loss of MEK due to the aldol reaction was only 4% to 5% due to the formation of 4gm to 5gm of 5-methyl-4-hepten-3-one as seen from GC-FID. The volume of the batch reactor used in the reaction was 250 ml, in which 125 ml of MEK was used.

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Abstract

The present application provides a process for the high yield production of methylpentenone (MPO) in a continuous mode by reacting an excess amount of methyl ethyl ketone (MEK) with acetaldehyde in the presence of a cation exchange resin catalyst in a fixed bed reactor having a plurality of sidewall injection ports, wherein acetaldehyde is injected from a plurality of sidewall injection ports of the reactor. The method also effectively reduces the complete consumption of the catalyst in the reaction process.

Description

technical field [0001] The present application relates to a method for producing methyl pentenone (methyl pentenone, MPO) in a continuous manner. In particular, the present application relates to a process for the production of methylpentenone (MPO) by reacting acetaldehyde with methyl ethyl ketone in the presence of a heterogeneous catalyst in a fixed bed reactor with a side wall injection port. Background technique [0002] Methylpent-3-en-2-one (MPO) is an important fine chemical used in the flavor and fragrance (Fragrance&Flavor, F&F) industry. Typically, MPO is produced industrially by the semi-batch aldol condensation reaction of methyl ethyl ketone (MEK) and acetaldehyde (AcH) in the presence of 98% sulfuric acid (catalyst). With current technological advancements, continuous production units offer advantages over traditional batch production. The global demand for MPO exceeds 25,000 tons per year, and with increasingly stringent environmental regulations, MPO produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C49/203B01J31/08B01J31/10
CPCC07C45/74B01J31/08B01J31/10B01J2231/342C07C49/203B01J8/025B01J8/0278B01J2208/00061B01J2208/00212C07C45/61B01J8/067B01J2208/00407B01J47/02B01J39/19
Inventor 苏米特·卡马尔拉凯什·狄隆桑杰·玛哈贾尼拉胡尔·纳巴拉维·南贾
Owner INDIAN INSTITUTE OF TECHNOLOGY BOMBAY
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