And Returning Distillation Product To A Previous Distillation Zone Patents (Class 203/78)
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Patent number: 7410556Abstract: The invention relates to a method and a device for the purification of an aqueous solution of an organic acid having a boiling point at atmospheric pressure of less than 450° C., which further has approximately 275 g carboxylate ions/1 or less, preferably 250 g carboxylate ions/1 or less, and preferably less than 1% by weight ionic impurities, calculated on the basis of the total solution. In particular, the invention relates to a method and a device for the continuous purification and concentration, on an industrial scale, of an aqueous solution of an organic acid having a boiling point at atmospheric pressure of less than 450° C. According to the method, this solution is subjected to two or more distillation steps, the first distillation step being carried out at a temperature of from 80° to 150° C. and a pressure of from 50 to 250 mbar, and the second distillation step being carried out at a temperature of from 80° to 200° C. and a pressure of from 0.01 to 50 mbar.Type: GrantFiled: November 27, 2000Date of Patent: August 12, 2008Assignee: Purac Biochem B.V.Inventors: Hendrik Martinus Winkelaar, Jan Van Breugel, Margarita Camprubi Vila, Jose Maria Vidal Lancis
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Patent number: 7384518Abstract: A method and a plant are disclosed for purifying lactams, particularly lactams obtained by cyclizing hydrolysis of aminonitrile. The purification of ?-caprolactam obtained by cyclizing hydrolysis of aminocapronitrile is described which includes eliminating the ammonia from the reaction medium of the hydrolysis, then recovering the lactam from said medium in purified form. The recovery is carried out by performing at least a distillation of the lactam in the presence of a base producing optionally a fronts fraction comprising compounds more volatile than the lactam, a fraction comprising the lactam to be recovered to the degree of desired purity and a distillation tails comprising the lactam and compounds less volatile than the lactam. The distillation tails are treated by various processes such as evaporation in thin layers to recover the major part of the caprolactam and recycling the latter in the purification process.Type: GrantFiled: May 28, 2001Date of Patent: June 10, 2008Assignee: Rhodia Polyamide IntermediatesInventors: Daniel Amoros, Philippe Leconte, Pierre Coqueret
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Patent number: 7351311Abstract: Crude water-containing tetrahydrofuran is purified by passing the crude tetrahydrofuran through three distillation columns, withdrawing water from the bottom of the first column, recycling water-containing tetrahydrofuran from the top of the second column into the first column, passing a sidestream of the first column into the second column, recycling the bottom product of the third column into the first column, and withdrawing a distillate at the top of the first column. Additionally, a sidestream of the second column is passed into the third column and the purified tetrahydrofuran is recovered as the top product of the third column.Type: GrantFiled: February 28, 2003Date of Patent: April 1, 2008Assignee: BASF AktiengesellschaftInventors: Gunther Windecker, Alexander Weck, Rolf-Hartmuth Fischer, Markus Rösch, Nils Bottke, Michael Hesse, Stephan Schlitter, Holger Borchert
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Patent number: 7339088Abstract: Improved processes and apparatus use a finishing column with a mid-cut that provides alkylbenzene products of high purity containing less than about 1 ppmw benzene and less than about 50 ppmw heavies while accommodating enhancements in the efficiencies and the capacities of the distillation train to recover alkylbenzene from alkylation reaction product and while enabling the use of catalytic treatments to reduce olefinic-component content.Type: GrantFiled: October 27, 2004Date of Patent: March 4, 2008Assignee: UOP LLCInventors: Dennis E. O'Brien, Douglas G. Stewart, Bipin V. Vora
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Patent number: 7329330Abstract: A process for working up by distillation the crude products obtained in the process according to DE-A 196 07 954 and containing 1,6-hexanediol (HDO), 1,5-pentanediol (PDO) or caprolactone (CLO) in order to obtain the corresponding pure products, the working-up by distillation being carried out in each case in a dividing wall column (TK) in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper common column region (1), a lower common column region (6), a feed section (2, 4) having a rectification section (2) and stripping section (4), and a take-off section (3, 5) having a stripping section (3) and rectification section (5), with feeding of the respective crude product HDO, PLO or CLO in the middle region of the feed section (2, 4) and removal of the high boiler fraction (C) from the bottom of the column, of the low boiler fraction (A) via the top of the column and of the medium boiler fraction (B) from the middle region of the take-off section (3, 5), orType: GrantFiled: January 8, 2002Date of Patent: February 12, 2008Assignee: Basf AktiengesellschaftInventors: Martin Gall, Gerd Kaibel, Thomas Krug, Harald Rust, Frank Stein
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Patent number: 7309403Abstract: The invention relates to a method of avoiding corrosion in the separation of methylamine from a product stream (10) which is obtained in the preparation of methylamines by gas-phase reaction of methanol and ammonia and includes monomethylamine, dimethylamine, trimethylamine, ammonia and methanol as components, where ammonia is separated off by pure distillation in a first column (1), the remaining components of the product stream obtained as bottoms (12) are fed to a second column (2). Trimethylamine (14) is separated off in the second column (2) by extractive distillation with introduction of water. The further of the product stream obtained as bottoms (15) from the second column (2) are fed to a third column (3), in which monomethylamine and dimethylamine are separated off at the top. The monomethylamine and dimethylamine are separated by distillation in a fourth column (4). To avoid corrosion alkali metal hydroxide is added to the second or third column (3).Type: GrantFiled: September 24, 2004Date of Patent: December 18, 2007Assignee: BASF AktiengesellschaftInventors: Werner Reutemann, Theodor Weber, Karl-Heinz Ross, Manfred Julius
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Patent number: 7169268Abstract: The present invention concerns a process for providing tertiary amine products which are color-stable, and have a greatly reduced tendency to take on color during their storage. According to the invention, an ethyleneamine derivative is added to the distillation pot prior to or during the distillation of the tertiary amine product. Preferably, the ethyleneamine derivative has a higher boiling point than the desired tertiary amine product so as to preclude the ethyleneamine from distilling over with the tertiary amine.Type: GrantFiled: June 6, 2003Date of Patent: January 30, 2007Assignee: Huntsman Petrochemical CorporationInventors: Wei-Yang Su, Mark L. Posey, Maarten P. ter Weeme
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Patent number: 7169267Abstract: A process is proposed for the separation of C5+ cuts by distillation into a low-boiler (A), a medium-boiler (B) and a high-boiler fraction (C) in one or more dividing-wall columns (TK), in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper, common column region (1), a lower, common column region (6), a feed part (2, 4) with rectifying section (2) and stripping section (4), and a withdrawal part (3, 5) with rectifying section (5) and stripping section (3), with feed of the C5+ cut (A, B, C) into the central region of the feed part (2, 4), discharge of the high-boiler fraction (C) from the bottom of the column, discharge of the low-boiler fraction (A) via the top of the column, and discharge of the medium-boiler fraction (B) from the central region of the withdrawal part (3, 5), wherein the dividing ratio of the liquid reflux at the upper end of the dividing wall (T) is set in such a way that the proportion of high-boiling key components in the liquid reType: GrantFiled: September 19, 2001Date of Patent: January 30, 2007Assignee: BASF AktiengesellschaftInventors: Gerd Kaibel, Carsten Oost, Manfred Stroezel, Gerald Meyer, Peter Trübenbach, Karl-Heinz Sartor, Jürgen Heners
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Patent number: 7157610Abstract: A process for recovering methanol from mixtures containing methanol and water, comprising multistage evaporation with heat integration, wherein the pressure is reduced from each stage to the next, and a downstream series of distillation stages with heat integration, wherein the pressure is increased from each stage to the next. The process reduces the amount of energy required for methanol recovery.Type: GrantFiled: December 19, 2005Date of Patent: January 2, 2007Assignees: Degussa AG, Uhde GmbHInventors: Willi Hofen, Thomas Haas, Bärbel Kolbe
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Patent number: 7147757Abstract: The invention relates to a method for separating by distillation a portion or the entirety of an azeptine derivative (III), which is selected from the group consisting of aminohexylidene imine, tetrahydroazepine, hexylhexahydroazepine and of aminohexylhexahydroazepine, out of a mixture (II) containing an azepine derivative (III) and an amine (I). The inventive method is characterized in that the distillation is carried out with a maximum bottom temperature of 150° C.Type: GrantFiled: March 6, 2001Date of Patent: December 12, 2006Assignee: Basf AktiengesellschaftInventors: Hermann Luyken, Frank Ohlbach
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Patent number: 7128813Abstract: A process for the high yield production of high purity glacial methacrylic acid (“HPMAA”) with minimization of decomposition of hydroxy isobutyric acid (HIBA). The HPMAA is substantially pure, specifically 99% pure or greater with a water content of 0.05% or less. This improved process involves the steps of providing a crude MAA stream which was formed by hydrolyzing acetone cyanohydrin and, therefore, includes HIBA which is an intermediate product of the hydrolysis reaction, and purifying that crude methacrylic acid stream in a series of successive distillation steps.Type: GrantFiled: April 22, 2003Date of Patent: October 31, 2006Assignee: Rohm and Haas CompanyInventors: Keith Frederick Briegel, James Clarence Day, Michael Stanley DeCourcy, Donald Alan Ebert, Jamie Jerrick John Juliette
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Patent number: 6998026Abstract: A tert-C4–C8-alkyl (meth)acrylate is prepared by reacting (meth)acrylic acid with an olefin of the formula where R1 and R2, which may be identical or different, are methyl or ethyl and R3 is H, methyl or ethyl, in homogeneous phase in the presence of an acidic catalyst and isolating the tert-C4–C8-alkyl (meth)acrylate from the reaction mixture, by a process in which the catalyst is separated off as residue by a two-stage distillation of the reaction mixture and the tert-C4–C8-alkyl (meth)acrylate is isolated from the distillates. The novel process makes it possible to use acetic acid-containing (meth)acrylic acid. The danger of cleavage of the ester and of polymerization of (meth)acrylic compounds is reduced.Type: GrantFiled: July 27, 2001Date of Patent: February 14, 2006Assignee: BASF AktiengesellschaftInventors: Ruprecht Kroker, Gerhard Nestler, Werner Schmitt, Winfried Schumm
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Patent number: 6986833Abstract: An amine-containing mixture containing one or more amines, water, low-boilers and optionally high-boilers is fractionated by a process having the steps (iii) and (iv) and optionally the steps (i), (ii) and (v): (i) a (first) low-boiler fraction is separated off from the amine-containing mixture by distillation, (ii) a (first) high-boiler fraction is separated off from the amine-containing mixture by distillation, (iii) the amine-containing mixture is extracted with sodium hydroxide solution, producing an aqueous, sodium-hydroxide-containing first phase and an aqueous-organic, amine-, (further) low-boiler- and possibly (further) high-boiler-containing second phase, (iv) the aqueous-organic second phase, is distilled, producing essentially anhydrous amine as bottom-phase take off or sidestream takeoff in the stripping part of the distillation column, an amine/water azeotrop as sidestream takeoff in the enrichment part of the column and a (further) low-boiler fraction as overhead takeoff, and recycling the aminType: GrantFiled: October 17, 2002Date of Patent: January 17, 2006Assignee: BASF AktiengesellschaftInventors: Andreas Wölfert, Heinz Rütter, Stefan Rittinger, Mark Wehinger, Aurelie Alemany, Willi Schmidt
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Patent number: 6982026Abstract: Disclosed herein are methods for the recovery of at least one of an organic acid or an organic acid amide, such as a heat stable lactic acid or lactamide, from a feed stream which contains the organic acid and/or organic acid amide. The feed stream is mixed with at least one azeotroping agent. The azeotroping agent is a hydrocarbon capable of forming at least one heteroazeotrope with the organic acid or the organic acid amide in the feed stream. The mixture of the feed stream and the azeotroping agent is heated to produce a vapor stream. The heteroazeotrope is a component of that vapor stream. The vapor stream can be heated further to separate components or it can be condensed into a liquid stream. The liquid stream is capable of being separated into a first phase and a second phase. The first phase contains the highest concentration of the organic acid and/or the organic acid amide and the azeotroping agent is part of the second phase.Type: GrantFiled: March 15, 2001Date of Patent: January 3, 2006Assignee: Tate & Lyle Ingredients Americas, Inc.Inventors: Michael Charles Milner Cockrem, Istvan Kovacs
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Patent number: 6972075Abstract: The invention relates to a method for removing, by distillation, 6-aminocapronitrile from mixtures that contain 6-aminocapronitrile, adipodinitrile and hexamethylenediamine, by a) removing the hexamethylenediamine from the mixture while obtaining a mixture (I) that has a hexamethylenediamine content of less than 1 wt. -%, b) removing completely or partially the 6-aminocapronitrile from mixture (I) while obtaining a mixture (II) whose content in substances that have a higher boiling point as 6-aminocapronitrile under distillation conditions and that cannot be formed by dimerization reactions when 6-aminocapronitrile is thermally treated is less than 1 wt. -%, and c) completely or partially removing from mixture (II) the hexamethylenediamine that might be present while obtaining a mixture (IV) whose hexamethylenediamine content is higher than that of mixture (II), and a mixture (V) whose hexamethylenediamine content is lower than that of mixture (II).Type: GrantFiled: June 13, 2001Date of Patent: December 6, 2005Assignee: BASF AktiengesellschaftInventors: Hermann Luyken, Frank Ohlbach, Rolf-Hartmuth Fischer, Johann-Peter Melder, Peter Bassler, Andreas Ansmann, Günther Achhammer
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Patent number: 6969446Abstract: Process for producing a nitric acid of a concentration from 75 to 99.9% from a more diluted nitric acid, wherein a nitric acid of a concentration of about 45 to 70% is rectified in contact with a liquid extraction medium to prevent the formation of a nitric acid-water-azeotropic mixture, and the vapors of the concentrated nitric acid are condensed and a concentrated nitric acid is obtained and wherein additionally the extraction medium is reconstituted through reconcentration and returned into the extractive rectification, wherein the nitric acid to be concentrated is fed as a boiling liquid or partially vaporized to the extractive rectification preferably carried out in two columns (K 1.0, K 1.Type: GrantFiled: May 22, 2000Date of Patent: November 29, 2005Assignee: QVF Engineering GmbHInventors: Gottfried Dichtl, Frank Dorstewitz, Manfred Sassenberg, Ulrich Walter
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Patent number: 6955743Abstract: The invention relates to a process for recovering and producing chemicals in a pulp production process where organic chemicals, such as formic acid and acetic acid, are used as cooking chemicals. The process of the invention is based on regeneration of cooking acids and formation of additional cooking acids and furfural by evaporating the cooking liquor and then separating acetic acid, formic acid, furfural and water. The separation is preferably carried out by distillation using the furfural formed in the process as a distilling aid in the distillation.Type: GrantFiled: December 28, 2001Date of Patent: October 18, 2005Assignee: Chempolis OyInventors: Esa Rousu, Pasi Rousu, Juha Anttila, Juha Tanskanen, Päivi Rousu
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Patent number: 6946060Abstract: A method to purify N,N-dimethylacetamide (DMAc) from an aqueous solution containing acetic acid as a contaminant. Two fractional distillation columns are arranged in a series. The solution containing the contaminant is provided to the first column with a temperature profile to result in acetic acid partitioning into the overhead water. The material remaining in the bottom portion of the first column is recycled to the first column and also provided into a second column, whereby DMAc free of acetic acid contamination is recovered, and remaining DMAc and acetic acid are returned to the first column for further separation. The method uses standard fractional distillation procedures and equipment, thus eliminating the need for more complex extractions and/or chromatographic separations.Type: GrantFiled: July 1, 2002Date of Patent: September 20, 2005Assignee: Mallinckrodt Inc.Inventor: Michael J. Gentilcore
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Patent number: 6913674Abstract: A mixture containing one or more amines, water, low-boilers and high-boilers, is fractioned in a process wherein (i) low-boilers are separated from the mixture by distillation, (ii) high-boilers are separated from the mixture by distillation, (iii) the mixture is extracted with a sodium hydroxide solution to form an aqueous, sodium-hydroxide-containing first phase and an aqueous-organic, amine-containing second phase, and (iv) the aqueous-organic second phase is distilled to form an amine/water azeotrop and an essentially anhydrous amine, and the amine/water azeotrop is recycled to the extraction step (iii).Type: GrantFiled: July 12, 2004Date of Patent: July 5, 2005Assignee: BASF AktiengesellschaftInventors: Andreas Wölfert, Heinz Rütter, Stefan Rittinger, Mark Wehinger, Aurelie Alemany, Willi Schmidt
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Patent number: 6896772Abstract: A process for distillative removal of ammonia from solutions (I) which include a lactam and ammonia comprises effecting said removal in a distillation apparatus (a) at an absolute pressure of less than 10 bar.Type: GrantFiled: June 2, 2001Date of Patent: May 24, 2005Assignee: BASF AktiengesellschaftInventors: Hermann Luyken, Frank Ohlbach, Stefan Maixner, Rolf-Hartmuth Fischer, Johann-Peter Melder, Peter Bassler, Andreas Ansmann
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Patent number: 6863778Abstract: A process for the separation of diisobutylene from tertiary butyl alcohol utilizing pressure swing azeotropic distillation to achieve the desired separation. The pressure swing azeotropic distillation takes advantage of the fact that different azeotropes are formed at different pressures. Isobutylene in C4 streams is oligomerized in the presence of tertiary butyl alcohol to produce the diisobutylene. Tertiary butyl alcohol is present in the dimerization because it improves the selectivity to the dimer (diisobutylene) by suppressing further reaction to the trimer or higher. The diisobutylene is separated from the tertiary butyl alcohol utilizing two distillation columns. The first distillation is operated at a higher pressure than the second such that the minimum boiling azeotropes of tertiary butyl alcohol and diisobutylene have different concentrations of tertiary butyl alcohol. Diisobutylene is removed as bottoms from the first distillation column and unreacted C4's are removed as overheads at 60-130 psig.Type: GrantFiled: December 9, 2002Date of Patent: March 8, 2005Assignee: Catalytic Distillation TechnologiesInventors: Jianhua Wang, Nishit Sahay, Mitchell E. Loescher, Montri Vichailak
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Patent number: 6849161Abstract: The present invention relates to a process for preparing anhydrous hydrazine. The process can include distilling an unconcentrated aqueous hydrazine solution into a starting binary solution, distilling the starting binary solution at a pressure where a concentration of hydrazine in the binary solution is greater than a concentration of an azeotrope at the distillation pressure, and recovering the anhydrous hydrazine.Type: GrantFiled: October 25, 2001Date of Patent: February 1, 2005Assignee: ArkemaInventor: Jean-Philippe Ricard
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Patent number: 6849162Abstract: A process for the preparation of propylene oxide in the presence of methanol, in which propylene oxide is separated from a mixture propylene oxide and methanol, and the resultant methanol containing mixture is worked up, including seperating methanol from a mixture comprising methanol and methyl formate during the work-up.Type: GrantFiled: July 5, 2001Date of Patent: February 1, 2005Assignee: BASF AktiengesellschaftInventors: Joaquim Henrique Teles, Alwin Rehfinger, Peter Bassler, Anne Wenzel, Norbert Rieber, Peter Rudolf
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Patent number: 6846389Abstract: In a process for the continuous fractional distillation of mixtures comprising tetrahydrofuran, ?-butyrolactone and/or 1,4-butanediol to give at least three fractions, the fractionation is carried out in an assembly of distillation columns comprising at least one dividing wall column or at least one assembly of thermally coupled conventional distillation columns.Type: GrantFiled: May 3, 2001Date of Patent: January 25, 2005Assignee: BASF AktiengesellschaftInventors: Gerd Kaibel, Alexander Weck, Ralf-Thomas Rahn
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Patent number: 6843890Abstract: A process of treating waste solvent acetonitrile streams which contain at least one water extractable impurity such as isopropyl acetate to remove substantially all of the impurity by distilling the waste solvent acetonitrile in the presence of water for a time sufficient to allow the water extractable impurity to be extractively distilled from the acetonitrile. In preferred embodiments of the present invention the feed may contain either a mixture of waste solvent acetonitrile and crude acetonitrile or crude acetonitrile free of hydrogen cyanide by itself.Type: GrantFiled: July 23, 1999Date of Patent: January 18, 2005Assignee: The Standard Oil CompanyInventor: Sanjay Purushottam Godbole
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Patent number: 6835287Abstract: An apparatus comprising first to third columns, wherein the outlet of a first column reboiler and the inlet of a second column condenser are connected by a first introduction conduit, and the outlet of a second distillation column reboiler and the inlet of a third column condenser are connected by a second introduction conduit, and additionally the outlet of the second column condenser and the inlet of the first column reboiler are connected by a first return conduit, and the outlet of the third column condenser and the inlet of the second column reboiler are connected by a second return conduit.Type: GrantFiled: October 11, 2000Date of Patent: December 28, 2004Assignee: Nippon Sanso CorporationInventors: Hitoshi Kihara, Hiroshi Tachibana, Shigeru Hayashida, Hiroshi Kawakami
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Patent number: 6821396Abstract: A mixture containing mixture one or more amines, water, low-boilers and high-boilers, is fractioned in a process wherein (i) low-boilers are separated from the mixture by distillation, (ii) high-boilers are separated from the mixture by distillation, (iii) the mixture is extracted with a sodium hydroxide solution to form an aqueous, sodium-hydroxide-containing first phase and an aqueous-organic, amine-containing second phase, and (iv) the aqueous-organic second phase is distilled to form an amine/water azeotrope and an essentially anhydrous amine, and the amine/water azeotrope is recycled to the extraction step (iii).Type: GrantFiled: October 17, 2002Date of Patent: November 23, 2004Assignee: BASF AktiengesellscahftInventors: Andreas Wolfert, Heinz Rütter, Stefan Rittinger, Mark Wehinger, Aurelie Alemany, Willi Schmidt
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Patent number: 6821382Abstract: A method and apparatus for cleaning condensate, produced during the production of cellulose pulp, including evaporation of spent liquor, utilizing a cleaning plant having several condensers, coupled in series. Process steam from the last evaporation stage and unclean condensate are introduced into a combined stripper/condenser, the process steam and the condensate being brought to flow in opposite directions so that direct heat exchange occurs, resulting in volatile compounds of the condensate being separated and taken up by the steam with simultaneous indirect cooling, resulting in condensation of the main part of the process steam, and the remaining process steam gradually flowing further on, the process steam being successively cooled first resulting in water and turpentine being condensed and collected and subsequently methanol being condensed.Type: GrantFiled: January 29, 2001Date of Patent: November 23, 2004Assignee: Papsea ABInventor: Allan Lundgren
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Publication number: 20040211657Abstract: A method of purifying 2,6-dimethylphenol to remove the odorous impurities includes distilling a crude mixture to yield a first light fraction enriched in 2,6-dimethylphenol, and a first heavy fraction enriched in 2,4,6-trimethylanisole, and distilling the first light fraction to yield a second light fraction, and a second heavy fraction enriched in 2,6-dimethylphenol. The concentration of 2,4,6-trimethylanisole in the second heavy fraction is less than 50% of the concentration of 2,4,6-trimethylanisole in the mixture. The purified 2,6-dimethylphenol is useful for preparing low-odor poly(arylene ether) resins.Type: ApplicationFiled: April 11, 2003Publication date: October 28, 2004Inventor: Hugo Gerard Eduard Ingelbrecht
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Publication number: 20040182752Abstract: This invention is an improved distillation sequence for the separation and purification of ethylene from a cracked gas. A hydrocarbon feed enters a C2 distributor column. The top of the C2 distributor column is thermally coupled to an ethylene distributor column, and the bottoms liquid of a C2 distributor column feeds a deethanizer column. The C2 distributor column utilizes a conventional reboiler. The top of the ethylene distributor is thermally coupled with a demethanizer column, and the bottoms liquid of the ethylene distributor feeds a C2 splitter column. The ethylene distributor column utilizes a conventional reboiler. The deethanizer and C2 splitter columns are also thermally coupled and operated at a substantially lower pressure than the C2 distributor column, the ethylene distributor column, and the demethanizer column. Alternatively, a hydrocarbon feed enters a deethanizer column.Type: ApplicationFiled: March 20, 2003Publication date: September 23, 2004Inventors: Rian Reyneke, Michael Foral, Christos G. Papadopoulos, Jeffery S. Logsdon, Wayne W. Y. Eng, Guang-Chung Lee, Ian Sinclair
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Publication number: 20040182693Abstract: There are disclosed an apparatus and a process for purification of an acrylic acid family.Type: ApplicationFiled: February 23, 2004Publication date: September 23, 2004Applicant: Nippon Shokubai Co., Ltd.Inventor: Yukihiro Matsumoto
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Patent number: 6793777Abstract: The invention relates to a method for separating and purifying an aqueous mixture that mainly consists of acetic acid, formic acid and high-boiling substances by extraction with a solvent in a cyclic process. The inventive method is characterized in that the flow of raffinate is fed to a solvent stripping column (11) with the major part of the water in order to remove the water from the cycle. The flow of extract is fed to a solvent recovery distillation column (8). In a first step, a mixture (A) that consists of water and solvent, is separated by overhead distillation. A mixture (B) that consists of acetic acid, formic acid and high-boiling substances is separated via a sump. Once the formic acid is removed in a column (29), mixture (B) is separated in an acetic acid distillation column to give pure acetic acid and high-boiling substances.Type: GrantFiled: December 5, 2001Date of Patent: September 21, 2004Assignee: Consortium für Elektrochemische Industrie GmbHInventors: Christoph Rüdinger, Harald Herbert Voit, Michael Hallmann, Mehmet Günaltay, Barbara Reil, Hans-Jürgen Eberle
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Patent number: 6758946Abstract: A process for working up hydroxylamine-containing solutions as obtained in particular in the electronics industry during the cleaning of electronic components is described. According to the invention, the hydroxylamine is stripped from the wastewater with steam. The products obtained are aqueous hydroxylamine and an aqueous solution of the amines. Both product streams can be purified in further process steps to give a saleable product.Type: GrantFiled: January 30, 2001Date of Patent: July 6, 2004Assignee: BASF AktiengesellschaftInventors: Otto Watzenberger, Heiner Schelling
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Publication number: 20040099522Abstract: The invention provides for the removal of impurities from treatment fluid comprising a base liquid and a variety impurities contained in the base liquid by conveying the treatment fluid to at least one preheating separating device, including a preheating heat exchanger and a separator unit, before the admixture of a carrier gas to the treatment fluid. The treatment fluid is preheated by the preheating heat exchanger to a temperature below the boiling temperature of a base liquid so that the liquid impurities with lower boiling temperatures than the base liquid are evaporated and expelled thermally, whereby the evaporated and expelled impurities are separated in the separator unit of the preheating separator device. The treatment fluid is then evaporated and separated from impurities having a lower boiling point than the base liquid.Type: ApplicationFiled: December 29, 2003Publication date: May 27, 2004Inventors: Joachim Neubert, Karl-Ferdinand Staab
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Publication number: 20040074758Abstract: The present invention provides a continuous process for recovering acetone from a waste stream from an acetone purification stage, whereas said waste stream comprises mesityl oxide and optionally acetone by separating the waste stream in a separating device at least in one stream comprising mesityl oxide and optionally a further stream comprising acetone, by than concentrating mesityl oxide in the mesityl oxide containing stream and finally by recycling the concentrated mesityl oxide stream to the separating device and bringing it into contact with a basic or acidic aqueous medium or with an acidic catalyst in the presence of water whereby mesityl oxide is at least partially hydrolyzed to acetone.Type: ApplicationFiled: July 3, 2003Publication date: April 22, 2004Inventors: Markus Weber, Otto Schnurr
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Publication number: 20040040829Abstract: A process for working up by distillation the crude products obtained in the process according to DE-A 196 07 954 and containing 1,6-hexanediol (HDO), 1,5-pentanediol (PDO) or caprolactone (CLO) in order to obtain the corresponding pure products, the working-up by distillation being carried out in each case in a dividing wall column (TK) in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper common column region (1), a lower common column region (6), a feed section (2, 4) having a rectification section (2) and stripping section (4), and a take-off section (3, 5) having a stripping section (3) and rectification section (5), with feeding of the respective crude product HDO, PLO or CLO in the middle region of the feed section (2, 4) and removal of the high boiler fraction (C) from the bottom of the column, of the low boiler fraction (A) via the top of the column and of the medium boiler fraction (B) from the middle region of the take-off section (3, 5), orType: ApplicationFiled: June 25, 2003Publication date: March 4, 2004Inventors: Martin Gall, Gerd Kaibel, Thomas Krug, Harald Rust, Frank Stein
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Patent number: 6695952Abstract: A method for the separation and purification of an aqueous mixture of main components, namely acetic acid and formic acid and non-volatiles by extraction, uses a solvent in a circulatory system. A raffinate stream is mixed with the larger proportion of water from a solvent stripper column (11) for the removal of water. The extraction stream is introduced into a solvent distillation column (8), from which in a first step involving the use of a mixture (A) containing a larger proportion of the solvent is separated out via a header and a mixture (B) of formic acid, water and solvent is separated out via a side offtake and a mixture (C) of acetic acid and non-volatiles is also separated out. A mixture (B) is introduced into a formic acid distillation column (4) for further processing, and a mixture (C) is introduced into an acetic acid distillation column (5), and purified acetic acid is subsequently isolated in the acetic acid distillation column (5) from the header.Type: GrantFiled: January 9, 2002Date of Patent: February 24, 2004Assignee: Consortium fur Elektrochemische Industrie GmbHInventors: Christoph Rüdinger, Harald Herbert Voit, Michael Hallmann, Mehmet Günaltay, Barbara Geborene Neé Reil Wild, Hans Jürgen Eberle
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Patent number: 6692616Abstract: A process is disclosed for the purification, by distillation, of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal, said process including the following steps: (a) reaction of n-butyraldehyde with formaldehyde in the presence of catalytic amounts of a tertiary amine, and hydrogenation of the resulting mixture to give a mixture containing trimethylolpropane; (b) separation of water, methanol, trialkylamine and/or trialkylammonium formate by distillation; (c) heating of the residue obtained in (b) under reduced pressure to a temperature at which TMP is volatile and compounds boiling above TMP are cleaved, in order to separate off, by distillation, TMP and compounds more volatile than TMP; (d) distillation of the distillate obtained in (c) in order to separate off the more volatile compounds and recover pure TMP; and (e) optional distillation of the TMP obtained in (d) in order to recover TMP with a low APHA color index.Type: GrantFiled: June 26, 2002Date of Patent: February 17, 2004Assignee: BASF AktiengesellschaftInventors: Matthias Dernbach, Detlef Kratz, Achim Stammer, Harald Rust, Gerhard Schulz
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Patent number: 6689251Abstract: A distiller (10) that employs a rotary heat exchanger (32) introduces water to be evaporated into evaporation chambers (56). During most of its operation, it collects the water that has passed through the evaporation chamber (56) without evaporating, and it reintroduces the thus-collected liquid back into the evaporation chamber, where it also adds a minor amount of unrecirculated feed liquid to make up for evaporation and concentrate removal. Simultaneously, a minor amount of feed liquid is fed into one side of a transfer pump (116). During this mode of operation, the impurities concentration in the recirculating liquid tends to increase as a result of the evaporation of pure water vapor. Periodically, the erstwhile recirculating liquid is redirected to the other side of the transfer pump (116), where it causes the feed liquid stored in the transfer pump's first side to be fed without accompanying recirculant liquid into the rotary heat exchanger's evaporation chambers.Type: GrantFiled: January 18, 2001Date of Patent: February 10, 2004Assignee: Ovation Products CorporationInventor: William H. Zebuhr
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Publication number: 20040020758Abstract: A process for the separation of diisobutylene from tertiary butyl alcohol utilizing pressure swing azeotropic distillation to achieve the desired separation. The pressure swing azeotropic distillation takes advantage of the fact that different azeotropes are formed at different pressures. Isobutylene in C4 streams is oligomerized in the presence of tertiary butyl alcohol to produce the diisobutylene. Tertiary butyl alcohol is present in the dimerization because it improves the selectivity to the dimer (diisobutylene) by suppressing further reaction to the trimer or higher. The diisobutylene is separated from the tertiary butyl alcohol utilizing two distillation columns. The first distillation is operated at a higher pressure than the second such that the minimum boiling azeotropes of tertiary butyl alcohol and diisobutylene have different concentrations of tertiary butyl alcohol. Diisobutylene is removed as bottoms from the first distillation column and unreacted C4's are removed as overheads at 60-130 psig .Type: ApplicationFiled: December 9, 2002Publication date: February 5, 2004Applicant: CATALYTIC DISTILLATION TECHNOLOGIESInventors: Jianhua Wang, Nishit Sahay, Mitchell E. Loescher, Montri Vichailak
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Patent number: 6685802Abstract: This invention relates to a continuous process and an apparatus (1) for removing dissolved and undissolved solids and/or high boiling point liquid contaminants from a mixture of miscible liquids (9). A recycle liquor stream (6) is fed at high velocity through a heat exchanger having a single flow path (12) and the heat added by the heat exchanger is sufficient to vaporize the feed stream (2) when the recycle liquor and feed stream are mixed upon delivery to the separation vessel (3).Type: GrantFiled: July 2, 2001Date of Patent: February 3, 2004Inventor: Craig Nazzer
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Patent number: 6679975Abstract: The present invention aims to isolate the azeotropes formed in a distillation column (B1) by methanol, propane and butane. The azeotropes are then liquefied in heat exchanger (E2) and mixed in contactor (M1) with water in order to dissolve the methanol in water. The mixture is then fed into a decantation tank (D2) to separate the aqueous phase from the liquid hydrocarbon phase. Finally, an aqueous phase containing methanol is discharged and the methanol-depleted hydrocarbon phase is recycled to distillation column (B1) as reflux.Type: GrantFiled: January 7, 2002Date of Patent: January 20, 2004Assignee: Institut Francais du PetroleInventors: Géraldine Laborie, Fabrice Lecomte, Annick Pucci
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Publication number: 20040000470Abstract: A method to purify N,N-dimethylacetamide (DMAc) from an aqueous solution containing acetic acid as a contaminant. Two fractional distillation columns are arranged in a series. The solution containing the contaminant is provided to the first column with a temperature profile to result in acetic acid partitioning into the overhead water. The material remaining in the bottom portion of the first column is recycled to the first column and also provided into a second column, whereby DMAc free of acetic acid contamination is recovered, and remaining DMAc and acetic acid are returned to the first column for further separation. The method uses standard fractional distillation procedures and equipment, thus eliminating the need for more complex extractions and/or chromatographic separations.Type: ApplicationFiled: July 1, 2002Publication date: January 1, 2004Applicant: MALLINCKRODT INC.Inventor: Michael J. Gentilcore
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Patent number: 6635151Abstract: The present invention relates to a process for separating the water from an aqueous lactam solution. It applies more particularly to a mixture resulting from the reaction between an aminonitrile and water (this reaction also being called cyclizing hydrolysis). The subject of the invention is a process for separating the water from an aqueous lactam solution, which process is economical both from the standpoint of the investment necessary for its implementation and from the standpoint of the operating cost.Type: GrantFiled: May 24, 2001Date of Patent: October 21, 2003Assignee: Rhodia Fiber & Resin IntermediatesInventors: Gerald Bocquenet, Yves Courtemanche, Patrick Houssier
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Patent number: 6632330Abstract: A process for the recovery of substantially pure alkyl alkanoate, such as ethyl acetate, from an impure feedstock. The impure feedstock is contacted with a selective hydrogenation catalyst in the presence of hydrogen in a selective hydrogenation zone maintained under selective hydrogenation conditions effective for selective hydrogenation of impurities containing reactive carbonyl groups thereby to hydrogenate the impurities to the corresponding alcohols. After recovery from the selective hydrogenation zone of a selectively hydrogenated reaction product mixture including the alkyl alkanoate and the corresponding alcohols, this is distilled in one or more distillation zones so as to produce substantially pure alkyl alkanoate therefrom which is recovered.Type: GrantFiled: June 5, 2001Date of Patent: October 14, 2003Assignee: Davy Process Technology LimitedInventors: Stephen William Colley, Norman Harris, Colin Rathmell
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Publication number: 20030183501Abstract: A distillation apparatus includes a column body; a partition for dividing the interior of the column body; a first distillation section composed of an enriching section and an exhaust section; a second distillation section composed of an enriching section formed above an upper end of the first distillation section, and an exhaust section located adjacent to the enriching section of the first distillation section; a third distillation section composed of an enriching section located adjacent to the exhaust section of the first distillation section, and an exhaust section formed below a lower end of the first distillation section; a condenser; a negative pressure generation system for generating a negative pressure to thereby withdraw vent gas; a gas cooler for cooling the vent gas; a first discharge system disposed at the side of the column body and adapted to discharge liquid rich in a medium-boiling-point component formed from a high-melting-point material; and a second discharge system disposed at the bottoType: ApplicationFiled: May 2, 2003Publication date: October 2, 2003Applicant: SUMITOMO HEAVY INDUSTRIES, LTD.Inventors: Katsunori Tamura, Yoichi Harada
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Patent number: 6605192Abstract: A process for the distillative recovery of high purity monoethylene glycol from the hydrolysis, product of ethylene oxide by pressure dewatering, preferably in a battery, vacuum dewatering and subsequent purifying distillation, wherein during the vacuum dewatering an aqueous stream is withdrawn which contains-monoethylene glycol in a concentration below 1% by weight, preferably below 0.1% by weight, medium boilers and low boilers. The withdrawn aqueous stream is, optionally after further workup, removed from the system.Type: GrantFiled: March 20, 2001Date of Patent: August 12, 2003Assignee: BASF AktiengesellschaftInventors: Gerhard Theis, Till Adrian, Bernd Bessling, Hans Hasse, Frans Vansant
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Patent number: 6605193Abstract: A method for isolating 32 from a crude mixture containing HCl and an azeotropic mixture of 32 and HF is provided without the need to isolate any HF azeotrope.Type: GrantFiled: April 25, 2001Date of Patent: August 12, 2003Assignee: Atofina Chemicals, Inc.Inventor: John A. Wismer
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Publication number: 20030146080Abstract: A process for the preparation of propylene oxide in the presence of methanol, in which propylene oxide is separated from a mixture comprising propylene oxide and methanol, and the resultant mixture comprising methanol is worked up, which comprises separating methanol from a mixture comprising methanol and methyl formate during the work-up.Type: ApplicationFiled: January 2, 2003Publication date: August 7, 2003Inventors: Joaquim Henrique Teles, Alwin Rehfinger, Peter Bassler, Anne Wenzel, Norbert Rieber, Peter Rudolf
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Patent number: 6599398Abstract: Process for the recovery of a purified adiponitrile (ADN) from a mixture of adiponitrile, aminocapronitrile and hexamethylenediamine, utilizing two sequential distillations: (1) a first distillation in which the mixture is distilled in a distillation column at a head pressure that causes at least 7% of the ADN to go into the distillate, along with bishexamethylenetriamine (BHMT) and 2-cyanocyclopentylideneimine (CPI), and (2) a second distillation in which the distillate from the first distillation is distilled in a second distillation column at a head pressure sufficient to cause minimum-temperature azeotropy between ADN and BHMT, thereby allowing the majority of the BHMT and CPI to be removed from the second distillation as distillate, and ADN, substantially free of both BHMT and CPI, to be removed as bottoms.Type: GrantFiled: July 17, 2002Date of Patent: July 29, 2003Assignee: E. I. du Pont de Nemours and CompanyInventors: John Ostermaier, Leon Scott, James Hastings