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    • 3. 发明专利
    • DK0934243T3
    • 2003-12-15
    • DK97912748
    • 1997-10-17
    • CELANESE INT CORP
    • SINGH MADANBLAY GEORGE AKARNILAW MICHAEL LMEILCHEN MELCHIOR APICARD WAYNE DAVIDSANTILLAN VALERIESCATES MARK OTANKE ROBIN SUZANNETORRENCE G PAULLVOGEL RICHARD F JRWARNER R JAY
    • B01J27/32B01J38/00C07C51/00C07C51/12C07C51/44C07C51/48C07C53/08C08G2/12C08G2/28
    • Disclosed is a method to manufacture high purity acetic acid. Although described in relation to that produced by a low water carbonylation process the present invention is applicable to other mechanisms for production of acetic acid which results in formation of permanganate reducing compounds such as acetaldehyde, propionic acid, and alkyl iodide impurities in intermediate process streams. It has been found that permanganate reducing compounds and alkyl iodides may be conveniently removed from a light phase of an intermediate stream in the reaction process by employing a multiple distillation process coupled with an optional extraction of acetaldehyde. The distillation process involves first distilling a light phase to concentrate the permanganate reducing compounds, and in particular the acetaldehyde, and then separating the permanganate reducing compounds and alkyl iodides in a second distillation tower. The second distillation serves to remove the permanganate reducing compounds and alkyl iodides from methyl iodide, methyl acetate, and methanol mixture. As an optional third step, the twice distilled stream may be directed to an extractor to remove any remaining quantities of methyl iodide from the aqueous acetaldehyde stream to obtain acetic acid as a final product in greater than 99% purity. It has been found that this process removes at least 50% of the permanganate reducing compounds and alkyl iodides and at least 20% of the propionic acid impurity from the intermediate light phase stream, and results in lower alkyl iodide concentration in the carbonylation reaction process, and in particular in the carbonylation reactor. It has also been found that during shut down of the inventive process, polymers of acetaldehyde tend to form in the base of the second distillation tower. To avoid or minimize the formation of these polymers, a constant flow of solvent is passed through the base of the column.
    • 9. 发明专利
    • AT247620T
    • 2003-09-15
    • AT97912748
    • 1997-10-17
    • CELANESE INT CORP
    • SINGH MADANBLAY GEORGE AKARNILAW MICHAEL LMEILCHEN MELCHIOR APICARD WAYNE DAVIDSANTILLAN VALERIESCATES MARK OTANKE ROBIN SUZANNETORRENCE G PAULLVOGEL RICHARD F JRWARNER R JAY
    • B01J27/32B01J38/00C07C51/00C07C51/12C07C51/44C07C51/48C07C53/08C08G2/12C08G2/28
    • Disclosed is a method to manufacture high purity acetic acid. Although described in relation to that produced by a low water carbonylation process the present invention is applicable to other mechanisms for production of acetic acid which results in formation of permanganate reducing compounds such as acetaldehyde, propionic acid, and alkyl iodide impurities in intermediate process streams. It has been found that permanganate reducing compounds and alkyl iodides may be conveniently removed from a light phase of an intermediate stream in the reaction process by employing a multiple distillation process coupled with an optional extraction of acetaldehyde. The distillation process involves first distilling a light phase to concentrate the permanganate reducing compounds, and in particular the acetaldehyde, and then separating the permanganate reducing compounds and alkyl iodides in a second distillation tower. The second distillation serves to remove the permanganate reducing compounds and alkyl iodides from methyl iodide, methyl acetate, and methanol mixture. As an optional third step, the twice distilled stream may be directed to an extractor to remove any remaining quantities of methyl iodide from the aqueous acetaldehyde stream to obtain acetic acid as a final product in greater than 99% purity. It has been found that this process removes at least 50% of the permanganate reducing compounds and alkyl iodides and at least 20% of the propionic acid impurity from the intermediate light phase stream, and results in lower alkyl iodide concentration in the carbonylation reaction process, and in particular in the carbonylation reactor. It has also been found that during shut down of the inventive process, polymers of acetaldehyde tend to form in the base of the second distillation tower. To avoid or minimize the formation of these polymers, a constant flow of solvent is passed through the base of the column.
    • 10. 发明专利
    • Acetic acid recovery system used for the iodide-promoted rhodium catalysed carbonylation of methanol to acetic acid
    • NZ334936A
    • 2000-10-27
    • NZ33493697
    • 1997-10-17
    • CELANESE INT CORP
    • SINGH MADANBLAY GEORGE AKARNILAW MICHAEL LMEILCHEN MELCHIOR APICARD WAYNE DAVIDSANTILLAN VALERIESCATES MARK OTANKE ROBIN SUZANNETORRENCE G PAULLVOGEL RICHARD FWARNER R JAY
    • B01J27/32B01J38/00C07C51/00C07C51/12C07C51/44C07C51/48C07C53/08C08G2/12C08G2/28B01D3/02
    • A process for reduction and/or removal of permanganate reducing compounds (PRC's) and C2-12alkyl iodide compounds formed in the carbonylation of methanol to a product of acetic acid, wherein said methanol is carbonylated in a suitable liquid phase reaction medium comprising a Group VIII metal catalyst, an organic iodide and iodide salt catalyst promoter; the products of carbonylation are separated into a volatile phase comprising product, and a less volatile phase comprising Group VIII metal catalyst, acetic acid, and iodide catalyst promoter; the product phase distilled in a distillation tower to yield a purified product and an overhead comprising organic iodide, methyl acetate, water, acetic acid, and unreacted methanol, directing at least a portion of the overhead to an overhead receiver decanter which separates the overhead into a light phase, comprising acetic acid and water, and a heavy phase comprising methyl acetate and organic iodide; and recycling the heavy phase to the carbonylation reactor, comprising the steps of: (a) Directing the light phase comprising acetic acid and water to a distiller which separates the mixture into two streams: residue stream comprising water and acetic acid and overhead stream comprising methyl iodide, methyl acetate, methanol, C2-12alkyl iodides, and PRC's; (b) Circulating the residue stream of step (a) to a heat exchanger and ultimately back to the reactor, and the overhead stream of step (a) to a second distiller which serves to strip the PRC's from the mixture. (c) Optionally forwarding the overhead stream containing PRC's of step (b) to an extractor to remove organic iodide compounds thereform; and, (d) Separating out concentrated PRC's for disposal and returning the organic iodide phase of (b) or (c) as a stream containing a lower percentage of PRC's and C2-12alkyl iodides to the carbonylation reactor. Figure 1 illustrates the removal of carbonyl impurities from the intermediate stream of the carbonylation process. Stream 28, comprising PRC's is directed to an overhead receiver decanter 16 where the light ends phase, stream 30, is directed to distillation column 18. The first vapour phase acetic acid stream (28) comprises methyl iodide, methyl acetate, acetaldehyde and other carbonyl components. This stream is then condensed and separated (in vessel 16) to form a first vapour phase stream to separate the heavy phase product containing the larger proportion of catalytic components - which is re-circulated to the reactor, and a light phase (30) comprising acetaldehyde, water, and acetic acid. This light phase is subsequently distilled twice to remove the PRC's and primarily the acetaldehyde component of the stream. The light phase (30) is directed to column 18, which serves to form a second vapour phase (36) enriched in aldehydes and alkyl iodides with respect to stream 28. Steam 36 is condensed (vessel 20) and bi-phasically separated to form a second heavy liquid phase product and a second light phase liquid product. This second heavy liquid phase contains a higher proportion of catalytic components than the second light liquid phase and is subsequently re-circulated to the reactor. The second liquid light phase (40) comprising acetaldehyde, methyl iodide, methanol, and methyl acetate is directed to a second distillation column (22) wherein the acetaldehyde is separated from the other components.