US2012245385A1PendingUtilityA1

Reactive distillation process and plant for obtaining acetic acid and alcohol from the hydrolysis of methyl acetate

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Assignee: SANDER STEFANPriority: Mar 25, 2011Filed: Mar 2, 2012Published: Sep 27, 2012
Est. expiryMar 25, 2031(~4.7 yrs left)· nominal 20-yr term from priority
C07C 51/44C07C 53/08B01J 19/32C07C 31/04B01D 3/009C07C 51/09C07C 29/80Y02P20/10C07C 29/147B01D 3/141C07C 51/487C07C 29/095C07C 29/88
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Claims

Abstract

Forming acetic acid and methanol from the hydrolysis of methyl acetate by reactive distillation is disclosed. A feed containing water and methyl acetate contacts a catalyst in a reactive space to perform the hydrolysis to form methanol and acetic acid. The reactive space comprises at least a first rectification zone, a first stripping zone and a first reaction zone. A catalyst is provided in the first reaction zone. The column further comprises a product space with at least a second rectification zone and a second stripping zone. The second stripping zone shares at least a portion of the column sump with the first stripping zone. A first head product is discharged from a reactive space head portion and a bottom product is discharged from the column sump and a second head product is discharged from a product space head portion and an intermediate product is discharged from the product space.

Claims

exact text as granted — not AI-modified
1 . A method for obtaining acetic acid and methanol from the hydrolysis of methyl acetate by reactive distillation in a reactive distillation column ( 1 ) which is configured as a divided wall reactive distillation column ( 1 ) including a column head ( 36 ), a column body ( 37 ) and a column sump ( 38 ) with the column body ( 37 ) being arranged between the column head ( 36 ) and the column sump ( 38 ), the column further comprises a reactive space ( 19 ) and a product space ( 29 ), wherein the reactive space ( 19 ) comprises at least a first rectification zone ( 32 ) and a first reaction zone ( 33 ), whereby a catalyst is provided in the first reaction zone ( 33 ) and the first rectification zone ( 32 ) is arranged between the column head ( 36 ) and the first reaction zone ( 33 ), the column further comprises a first stripping zone ( 34 ), with the first stripping zone ( 34 ) being arranged between the column sump ( 38 ) and the first reaction zone ( 33 ), wherein the product space ( 29 ) comprises at least a second rectification zone ( 42 ) and a second stripping zone ( 44 ), whereby a feed containing water and methyl acetate enters the reactive space ( 19 ) and is brought into contact with the hydrolysis catalyst to be at least partially hydrolysed to acetic acid and methanol, characterised in that the second stripping zone ( 44 ) shares at least a portion of the column sump ( 38 ) with the first stripping zone ( 34 ) and a first head product is discharged from a reactive space head portion ( 45 ) and a bottom product is discharged from the column sump ( 38 ) and a second head product is discharged from a product space head portion ( 46 ) and an intermediate product is discharged from the product space ( 29 ). 
     
     
         2 . The method of  claim 1 , wherein the methanol and methyl acetate in the bottom product amount to less than 1%, preferably less than 0.5% particularly preferred less than 0.1%. 
     
     
         3 . The method of  claim 1 , wherein the second head product substantially consists of methanol and methyl acetate. 
     
     
         4 . The method of  claim 3 , wherein the impurities in the second head product amount to less than 1%, preferably less than 0.5% particularly preferred less than 0.1%. 
     
     
         5 . The method of  claim 1 , wherein a pre-reactor feed containing methyl acetate is firstly fed to a pre-reactor ( 2 ), in which the methyl acetate is brought into contact with a hydrolysis catalyst in the presence of water, by means of which the methyl acetate is partially cleaved into acetic acid and methanol and a pre-reactor product containing methyl acetate, acetic acid and methanol is discharged from the pre-reactor ( 2 ) and is fed as the first feed into the reactive distillation column. 
     
     
         6 . A methyl acetate hydrolysis plant for obtaining acetic acid and methanol through the hydrolysis of methyl acetate by reactive distillation includes a divided wall reactive distillation column ( 1 ) including a column head ( 36 ), a column body ( 37 ) and a column sump ( 38 ) and the column body ( 37 ) being arranged between the column head ( 36 ) and the column sump ( 38 ), the column further comprising a reactive space ( 19 ) and a product space ( 29 ), and a wall ( 5 ) arranged in parallel to the longitudinal axis ( 35 ) of the column, said wall ( 5 ) dividing the column into the reactive space ( 19 ) and the product space ( 29 ), wherein the reactive space ( 19 ) comprises at least a first rectification zone ( 32 ) and a first reaction zone ( 33 ) with a catalyst being provided in the first reaction zone ( 33 ), wherein the first rectification zone ( 32 ) is arranged between the column head ( 36 ) and the first reaction zone ( 33 ), the column further comprising a first stripping zone ( 34 ), with the first stripping zone ( 34 ) being arranged between the column sump ( 38 ) and the first reaction zone ( 33 ), wherein the product space ( 29 ) comprises at least a second rectification zone ( 42 ) and a second stripping zone ( 44 ), characterised in that the second stripping zone ( 44 ) shares at least a portion of the column sump ( 38 ) with the first stripping zone ( 34 ). 
     
     
         7 . The methyl acetate hydrolysis plant of  claim 6 , wherein a sump conduit ( 16 ) is provided for drawing off a bottom product from the column sump ( 38 ), said bottom product substantially consisting of acetic acid and water. 
     
     
         8 . The methyl acetate hydrolysis plant of  claim 6 , wherein a first head discharge conduit ( 18 ) is provided for drawing off a first head product from a reactive space column head portion ( 45 ) and a second head discharge conduit ( 28 ) is provided for drawing off a second head product from the product space column head portion ( 46 ), said second head product consisting substantially of methanol and methyl acetate. 
     
     
         9 . The methyl acetate hydrolysis plant of  claim 8 , wherein a first condenser ( 30 ) is foreseen for condensing a portion or all of said first head product and a second condenser ( 31 ) is foreseen for condensing a portion or all of said second head product. 
     
     
         10 . The methyl acetate hydrolysis plant of  claim 9 , wherein a first reflux conduit ( 24 ) is provided for recycling a portion of said first head product to the reactive space ( 19 ) and a second reflux conduit ( 24 ) is provided for recycling a portion of said second head product to the product space ( 29 ). 
     
     
         11 . The methyl acetate hydrolysis plant of  claim 6 , wherein a first feed conduit ( 14 ) for a first feed containing water and a second feed conduit ( 15 ) for a second feed containing methyl acetate are provided to enter the column ( 1 ) on the reactive space ( 19 ) thereof. 
     
     
         12 . The methyl acetate hydrolysis plant of  claim 6 , wherein a pre-reactor feed conduit ( 3 ) for a pre-reactor feed containing methyl acetate and water to a pre-reactor ( 2 ) is provided, the pre-reactor ( 2 ) containing a hydrolysis catalyst, by means of which the methyl acetate is partially cleavable into acetic acid and methanol and a pre-reactor product containing methyl acetate, acetic acid and methanol from the pre-reactor is provided to be fed to the second feed conduit ( 15 ) to the divided wall reactive distillation column ( 1 ). 
     
     
         13 . Use of a structured packing or trays in the reaction zone of a methyl acetate hydrolysis plant of  claim 6  which can comprise a hydrolysis catalyst provided on the surfaces of a structured packing, which can form a structured catalyst packing. 
     
     
         14 . Use of a structured packing according to  claim 13 , whereby the structured catalyst packing comprises at least one retaining device. 
     
     
         15 . Use of a structured packing according to  claim 14 , wherein the retaining device comprises at least one of a bag for solid catalyst material or a flow channel.

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