Purification Or Recovery Per Se Patents (Class 562/600)
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Patent number: 6627047Abstract: A method is provided for preventing an easily polymerizable substance from being polymerized in a thin-film type evaporating device by supplying a solution of the substance to the evaporating heating surface of the device by the centrifugal force of a stirring rotary shaft, characterized by mixing a distilled vapor of the substance with a molecular oxygen-containing gas and supplying the extracted liquid or a solution having lower viscosity than the extracted liquid to a feed raw material inlet thereby adjusting the quantity of a wetting liquid per unit length of the surface in the range of 0.02-2 m3/mHr. In the evaporation of the substance by the use of the device, a method for preventing the substance from polymerization is provided.Type: GrantFiled: April 21, 2000Date of Patent: September 30, 2003Assignee: Nippon Shokubai Co., Ltd.Inventors: Yuichi Ijiri, Takeshi Nishimura, Yukihiro Matsumoto
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Patent number: 6620969Abstract: A shell-and-tube heat exchanger for handling an easily polymerizable substance is disclosed, which is characterized by having no part for stagnation of said process fluid on the surfaces for contact with the process fluid. By eliminating undulations from the inner surfaces of the heat transfer tubes, it is made possible to prevent the easily polymerizable substance from polymerizing and, at the same time, prevent adhesion of a polymer to the surfaces. Thus, the efficiency of heat exchange is enhanced and the protracted continuous operation is realized.Type: GrantFiled: March 8, 2000Date of Patent: September 16, 2003Assignee: Nippon Shokubai Co. , Ltd.Inventors: Takeshi Nishimura, Yukihiro Matsumoto
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Patent number: 6613196Abstract: A method for stopping a purifying column handling an easily polymerizing compound-containing solution is disclosed, which method is characterized by lowering the inner oxygen concentration of the column below the limit of oxygen concentration by supplying an inert gas to the column while the concentration of the gas of easily polymerizing compound is in the range of 100% to the lower limit of the flammable range in volume % of the purifying column or by further supplying a reflux liquid thereby cooling the interior of the column at a rate in the range of 0.01-10° C./min. This invention enjoys exceptionally high economic value in respect that it is capable of preventing the easily polymerizing compound from the occurrence of polymerization in the purifying column, precluding the interior of the purifying column from being clogged by adhesion of a polymer, and moreover avoiding the possibility of explosion.Type: GrantFiled: July 9, 2001Date of Patent: September 2, 2003Assignee: Nippon Shokubai Co., Ltd.Inventors: Kei Hamamoto, Yukihiro Matsumoto, Sei Nakahara, Misao Inada
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Publication number: 20030150705Abstract: A method of recovering acrylic acid from a mixture comprising acrylic acid, water and acetic acid is disclosed, which includes:Type: ApplicationFiled: December 30, 2002Publication date: August 14, 2003Inventors: Sanjeev D. Deshpande, Tao Wang, Olan Stanley Fruchey, Roger L. Roundy, Nathan K. Powell, Rafael G. Morales, Joseph E. Goins
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Publication number: 20030146081Abstract: A method of recovering acrylic acid from a mixture comprising acrylic acid, water and acetic acid is disclosed, which includes: (a) extracting acrylic acid from the mixture with a solvent mixture comprising ethyl acrylate as the preponderant component thereof and an organic co-solvent selected from the group consisting of toluene, heptane, 1-heptene, methylcyclohexane, cycloheptane, cycloheptadiene, cycloheptatriene, 2,4-dimethyl-1,3 pentadiene, methylcyclohexene and methylenecyclohexene to form an extracted composition; and (b) azeotropically distilling the extracted composition to recover acrylic acid.Type: ApplicationFiled: January 8, 2002Publication date: August 7, 2003Inventors: Salvador Aldrett, Diane Elizabeth Allen, Nathan K. Powell, Christopher Lawrence Wilkins, Edmund Jungpiao Yang
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Publication number: 20030149301Abstract: Crude acrylic acid is purified batchwise by crystallization by a process which comprises at least one purification stage and at least one stripping stage and in which at least the first stripping stage is carried out in a different crystallizer from the first purification stage.Type: ApplicationFiled: November 12, 2002Publication date: August 7, 2003Inventors: Bernd Eck, Dieter Baumann, Jorg Heilek, Klaus Joachim Muller-Engel
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Patent number: 6596129Abstract: The present invention provides: a process can be preventive of a polymerization in a distillation apparatus when distilling a solution containing easily polymerizable substances such as (meth)acrylic acid and (meth)acrylic acid ester. In the distillation process for an easily polymerizable substance-containing solution which includes the step of distilling an easily polymerizable substance-containing solution by a distillation column equipped with a condenser for condensation at a vapor outlet of the distillation column, at least one condenser for polymerization inhibition is further placed in series on a vapor outlet side of the condenser for condensation, and the easily polymerizable substance which is contained in vapor from an upstream condenser is condensed by a downstream condenser.Type: GrantFiled: October 31, 2000Date of Patent: July 22, 2003Assignee: Nippon Shokubai Co., Ltd.Inventors: Yukihiro Yoneda, Takeshi Nishimura, Yasuhiro Shingai, Hajime Matsumoto
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Patent number: 6596901Abstract: A process for preparing acrylic acid or methacrylic acid comprises (a) preparing a gaseous product mixture having essentially the composition of a reaction mixture of the catalytic gas phase oxidation of C3-/C4-alkanes, -alkenes, -alkanols and/or -alkanals and/or precursors thereof to form acrylic acid or methacrylic acid, characterized by (b) condensing said product mixture, (c) crystallizing acrylic acid or methacrylic acid from the solution obtained in step (b), and (d) removing the resulting crystals from the mother liquor.Type: GrantFiled: January 8, 1999Date of Patent: July 22, 2003Assignee: BASF AktiengesellschaftInventors: Bernd Eck, Otto Machhammer, Theo Proll, Volker Schliephake, Klaus Joachim Müller-Engel
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Publication number: 20030127315Abstract: A tert-C4-C8-alkyl (meth)acrylate is prepared by reacting (meth)acrylic acid with an olefin of the formula 1Type: ApplicationFiled: January 27, 2003Publication date: July 10, 2003Inventors: Ruprecht Kroker, Gerhard Nestler, Werner Schmitt, Winfried Schumm
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Publication number: 20030121768Abstract: A process for the separation and purification of acrylic acid is disclosed, wherein ethyl propionate is employed as an extraction solvent.Type: ApplicationFiled: December 13, 2001Publication date: July 3, 2003Inventors: Salvador Aldrett Lee, Diane Elizabeth Allen, Christopher Lawrence Wilkins
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Patent number: 6585862Abstract: The present invention provides an apparatus for handling an easily polymerizable compound such as (meth)acrylic acid which includes a tubular member that is furnished to a side wall of the apparatus and opened to the inside of the apparatus, specifically, for example, an apparatus and a method which effectively inhibit the polymerization of (meth)acrylic acid in a distillation column for (meth)acrylic acid wherein the distillation column has such as an inlet or outlet of gas or liquid, a manhole, or a tube into which an instrument is inserted. The tubular member (e.g. an inlet or outlet, a manhole, a tube into which an instrument is inserted) is set so as to have a downward gradient (&agr;) in the range of 3° to 70° toward the inside of the apparatus.Type: GrantFiled: August 19, 2000Date of Patent: July 1, 2003Assignee: Nippon ShokubaiInventors: Takeshi Nishimura, Yukihiro Matsumoto
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Publication number: 20030120112Abstract: The object of the present invention is to provide a method to suppress changes the concentration of (meth)acrylic acid in the bottom solution discharged from the absorption column, and to enable stable operation for separating and purifying (meth)acrylic acid in the subsequent steps onward.Type: ApplicationFiled: November 27, 2002Publication date: June 26, 2003Inventor: Harunori Hirao
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Publication number: 20030092937Abstract: Economical processes are disclosed for recovery and refining of at least acrylic acid from a gaseous mixture such as is obtainable by gas-phase catalytic oxidation of propylene. Processes of the invention include quenching the gaseous mixture with an aqueous quench liquid to obtain an aqueous solution comprising the acid values; contacting the aqueous solution with an immiscible extraction solvent; and an integrated sequence of distillations and phase separations to recover for recycle organic components of the extraction solvent, and obtain valuable acrylic acid and acetic acid products. Advantageously, the immiscible extraction solvent is substantially free of aromatic compounds such as benzene and toluene.Type: ApplicationFiled: November 13, 2001Publication date: May 15, 2003Inventors: David R. Wagner, Steve J. Miko
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Publication number: 20030092938Abstract: A method of manufacturing (meth)acrylic acid includes:Type: ApplicationFiled: December 20, 2002Publication date: May 15, 2003Inventors: Takeshi Nishimura, Yukihiro Matsumoto
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Patent number: 6555707Abstract: A process for preparing acrylic acid and/or acrylates, which comprises stage A with or without stages B and C: A: cooling a gaseous reaction mixture which comprises acrylic acid and is obtained in the gas-phase oxidation to prepare acrylic acid, using an inert high-boiling solvent, to give a gaseous mixture comprising acrylic acid; B: separating the gaseous mixture comprising acrylic acid to give a low-boiling fraction, a crude acrylic acid, and a bottom product, and C: esterifying the crude acrylic acid obtained in stage B by means of one or more alkanols to give an esterification mixture comprising one or more acrylates and one or more acetic esters.Type: GrantFiled: September 22, 2000Date of Patent: April 29, 2003Assignee: BASF AktiengesellschaftInventors: Gerhard Nestler, Jürgen Schröder, Gerhard Bolz
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Publication number: 20030065215Abstract: An object of this invention is to provide a method for producing acrylic acid that enables to suppress adverse influence of byproducts during distillation and to accomplish long-term continuous operation of the acrylic acid production apparatus. This invention is directed to a method for producing (meth)acrylic acid comprising the step of isolating (meth)acrylic acid from a liquid containing (meth)acrylic acid by distillation wherein the liquid contains glyoxal (including its hydrate) in a concentration of 0.1 mass % or less.Type: ApplicationFiled: September 26, 2002Publication date: April 3, 2003Inventors: Kazuhiko Sakamoto, Kazuo Ohkouchi, Tomohiro Nakae
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Publication number: 20030062253Abstract: The object of this invention to provide an improved arrangement that enables to prevent adhesion of polymer on or around the inner wall of a purification apparatus directly equipped on the outer wall thereof with an attachment such as a support by suppressing local temperature lowering inside the apparatus due to the existence of the attachment. The present invention provides a purification apparatus comprising an attachment directly mounted on an outer wall of the apparatus; and a covering material made of a low heat conductive material which partly or entirely covers the outer wall of the apparatus, and which partly or entirely covers the attachment.Type: ApplicationFiled: September 26, 2002Publication date: April 3, 2003Inventors: Yukihiro Matsumoto, Takeshi Nishimura
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Patent number: 6541665Abstract: In a process for the purification of acrylic acid or methacrylic acid by crystallization and distillation, the following steps are carried out: (a) crystallization of a mixture containing the acrylic acid or methacrylic acid with formation of product crystals having a higher concentration of acrylic acid or methacrylic acid and of a mother liquor, (b) distillation of at least part of the mother liquor from step (a) with formation of a distillation residue, which is at least partly removed, and of a top product, (c) crystallization of at least part of the top product from step (b) with formation of a crystallization residue, which is removed, and of crystals and (d) recycling of the crystals from step (c) to the crystallization (a).Type: GrantFiled: January 2, 2001Date of Patent: April 1, 2003Assignee: BASF AktiengesellschaftInventors: Erik Bastiaensen, Bernd Eck, Joachim Thiel
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Patent number: 6540881Abstract: This invention relates to a method for preventing (meth)acrylic acid from polymerizing during the course of distillation. The method provides for refining (meth)acrylic acid by a procedure including the steps of feeding a mixed gas obtained by catalytic gas phase oxidation of propylene and/or acrolein with a molecular oxygen-containing gas or a mixed gas obtained by catalytic gas phase oxidation of at least one compound of isobutylene, t-butyl alcohol, or methacrolein with a molecular oxygen-containing gas, to a (meth)acrylic acid collection column, collecting a (meth)acrylic acid-containing solution from the mixed gas, and feeding the (meth)acrylic acid-containing solution to a distillation column while maintaining the total concentration of aldehydes of 2-4 carbon atoms and acetone in the solution at a level of not more than 2000 ppm based on the amount of (meth)acrylic acid.Type: GrantFiled: March 22, 2000Date of Patent: April 1, 2003Assignee: Nippon Shokubai Co., Ltd.Inventors: Kazuhiko Sakamoto, Kouji Ueno, Sei Nakahara, Masatoshi Ueoka
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Publication number: 20030060661Abstract: In a process for the purification of a crude acrylic acid melt, the crude acrylic acid melt is converted, under the action of low temperatures, into a crude acrylic acid suspension consisting of acrylic acid crystals and residual melt, and the acrylic acid crystals of the crude acrylic acid suspension are freed from remaining residual melt in a wash column, the production of the acrylic acid crystals of the crude acrylic acid suspension being carried out in the presence of water, the wash column being a wash column with forced transport of the acrylic acid crystals and the wash liquid used being the melt of acrylic acid crystals purified in the wash column.Type: ApplicationFiled: October 1, 2002Publication date: March 27, 2003Inventors: Bernd Eck, Dieter Baumann, Jorg Heilek, klaus Joachim Muller-Engel
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Patent number: 6525216Abstract: A method of manufacturing (meth)acrylic acid includes: a reaction step of carrying out a catalytic gas-phase oxidation reaction; an absorbing step of absorbing (meth)acrylic acid from a (meth)acrylic-acid-containing mixed gas prepared in the reaction step; a refinement step of separating, refining, and recovering (meth)acrylic acid from a (meth)acrylic-acid-containing liquid prepared in the absorbing step; and a recirculation step of recirculating (meth)acrylic acid contained in a vent gas produced in the refinement step to the absorbing step and/or the refinement step.Type: GrantFiled: June 7, 2000Date of Patent: February 25, 2003Assignee: Nippon Shokubai Co., Ltd.Inventors: Takeshi Nishimura, Yukihiro Matsumoto
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Publication number: 20030028052Abstract: This invention concerns a method for absorbing acrylic acid, characterized by supplying an acrylic acid-containing reaction gas component obtained by the reaction of catalytic gas phase oxidation to an acrylic acid absorption column and advancing a high boiling inert hydrophobic organic liquid into counter-flow contact with said reaction gas in said acrylic acid absorption column with the mass flow rate of the organic liquid fixed in the range of 0.2-7.0 times the mass flow rate of the acrylic acid in the reaction gas thereby absorbing acrylic acid in said organic liquid and obtaining an acrylic acid-containing solution including a low boiling substance in the range of 0.7-7.5 wt % based on the weight of bottom liquid of absorption column.Type: ApplicationFiled: August 2, 2002Publication date: February 6, 2003Inventors: Harunori Hirao, Yoshitake Ishii, Yukihiro Matsumoto, Takeshi Nishimura
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Patent number: 6515171Abstract: An oxidation reaction mixture (e.g. adipic acid, benzoic acid, butenediol) and an oxidation catalyst are efficiently separated from a reaction mixture with the use of an aqueous solvent (e.g. methyl benzoate, benzonitrile) containing at least water (e.g. water) and a non-water-soluble solvent separable from the aqueous solvent, the reaction mixture being obtained by oxidizing a substrate (e.g. a hydrocarbon) in the presence of an imide compound such as N-hydroxyphthalimide shown by the following formula (1) as the oxidation catalyst, wherein R1 and R2 represents a substituent such as a hydrogen atom and a halogen atom; R1 and R2 may together form a double bond, or an aromatic or nonaromatic 5- to 12-membered ring; X stands for O or OH; and n is 1 to 3. No decomposition of the oxidation catalyst is observed in this separation process.Type: GrantFiled: August 15, 1997Date of Patent: February 4, 2003Assignee: Daicel Chemical Industries, Ltd.Inventor: Naruhisa Hirai
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Publication number: 20030018214Abstract: (Meth)acrylic acid is purified by crystallization by a process in which the (meth)acrylic acid is purified by a combination of at least two different dynamic crystallization processes, in particular a suspension crystallization and a layer crystallization.Type: ApplicationFiled: July 26, 2002Publication date: January 23, 2003Inventors: Emile De Decker, Erik Bastiaensen, Dieter Baumann, Bernd Eck, Jorg Heilek
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Patent number: 6509498Abstract: The invented process produces sorbic acid or its salt through the decomposition of a polyester obtained from ketene and aldehyde, and includes the step of treating a solution containing-sorbic acid or its salt with a chemically activated carbon, which sorbic acid or its salt is produced by the decomposition of the polyester. The treatment with activated carbon is performed, for example, at pH ranging from 5.8 to 7.5 at temperatures ranging from 30° C. to 80° C. The invented process can efficiently remove colored substances and can easily yield a high quality sorbic acid having a satisfactory hue in a high yield.Type: GrantFiled: May 26, 2000Date of Patent: January 21, 2003Assignee: Daicel Chemical Industries, Ltd.Inventors: Akira Yamashita, Mitsuhiro Kouno
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Patent number: 6504056Abstract: A method of transporting and/or storing pure acrylic acid comprises ensuring by means of appropriate measures that the pure acrylic acid is partly crystalline during the entire duration of transport and/or storage.Type: GrantFiled: May 1, 2001Date of Patent: January 7, 2003Assignee: BASF AktiengesellschaftInventors: Heinrich Aichinger, Gerhard Nestler, Paul Leon Kageler
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Patent number: 6500982Abstract: This invention relates to a process for preparing (meth)acrylic acid, whereby turndown control is utilized to maintain optimal distillation column performance in the dehydration of aqueous (meth)acrylic acid to provide a (meth)acrylic acid solution.Type: GrantFiled: June 13, 2000Date of Patent: December 31, 2002Assignee: Rohm and Haas CompanyInventors: Timothy Allen Hale, Robert Michael Mason, Josefina Tseng Chapman, James Clarence Day, Chorng-Shyuan Tsay
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Patent number: 6498272Abstract: In a process for the preparation of acrylic acid, a product gas mixture obtained by catalytic gas-phase oxidation of a C3-precursor of acrylic acid and containing acrylic acid is directly cooled with a quench liquid and then subjected to fractional condensation in a separation column provided with baffles, said product gas mixture ascending into itself and a crude acrylic acid being removed via a side take-off, and the acrylic acid oligomers formed are cleaved and recycled.Type: GrantFiled: August 30, 2001Date of Patent: December 24, 2002Assignee: BASF AktiengesellschaftInventors: Jürgen Schröder, Gerhard Nestler, Klaus Joachim Müller-Engel
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Publication number: 20020189927Abstract: The present invention provides a column treating method by use of a distillation column and so on, which method enables to effectively remove solid impurities such as precipitates and polymers contained or produced in a treating fluid, and to thereby stably operate the column treatment. Solid impurities in a treating fluid can be removed by carrying out: step (a) of drawing out the treating fluid from a drawing out outlet (16) at the column bottom of the treatment column (10) outside the treatment column (10), step (b) of removing solid impurities from the treating fluid, drawn out in step (a), by a strainer (40), and step (c) of returning the treating fluid, from which the solid impurities are removed in step (b), to a returning inlet (18) of the treatment column, with advancing physical and/or chemical treatment of the treating fluid in the treatment column (10).Type: ApplicationFiled: August 22, 2002Publication date: December 19, 2002Applicant: Nippon Shokubai Co., Ltd.Inventors: Kazuhiko Sakamoto, Sei Nakahara, Masatoshi Ueoka, Naoto Kasaya
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Patent number: 6482981Abstract: A method of producing highly purified acrylic acid in a high yield is provided. A method of producing acrylic acid including the steps of an oxidation step, an absorption step, a distillation step, a crystallization step, and a dimer decomposition step.Type: GrantFiled: January 3, 2001Date of Patent: November 19, 2002Assignee: Nippon Shokubai Co., Ltd.Inventors: Kouji Ueno, Masatoshi Ueoka, Sei Nakahara
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Patent number: 6458989Abstract: A process for preparing pure (meth)acrylic acid or a (meth)acrylate starting from a crude (meth)acrylic acid, which comprises the following stages: A: treating the crude (meth)acrylic acid with at least one compound which is able to remove aldehydes, to give an aldehyde-free crude (meth)acrylic acid; B: subjecting the aldehyde-free crude (meth)acrylic acid to imprecise distillation, to give a low-boiling fraction comprising (meth)acrylic acid and acetic acid and a high-boiling fraction comprising (meth)acrylic acid and high boilers; C: isolating a pure (meth)acrylic acid from the high-boiling fraction and, if desired, D: esterifying the low-boiling fraction comprising (meth)acrylic acid and acetic acid that is obtained in stage B by means of one or more alkanols, to give an esterification mixture comprising one or more (meth)acrylates, one or more acetic esters, and one or more alkanols.Type: GrantFiled: September 28, 2000Date of Patent: October 1, 2002Assignee: BASF AktiengesellschaftInventors: Heinrich Aichinger, Hans Martan, Gerhard Nestler
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Publication number: 20020134660Abstract: A method for distilling a raw material liquid containing (meth)acrylic acid substantially free from azeotropic solvents, collected with a collection agent from a mixed gas obtained by gas phase catalytic oxidation reactions which includes feeding to a distillation column the raw material liquid which temperature is substantially equal to that of the entrance place in the column.Type: ApplicationFiled: March 1, 2002Publication date: September 26, 2002Inventors: Kazuhiko Sakamoto, Sei Nakahara, Yukihiro Matsumoto, Kenji Sanada, Masatoshi Ueoka
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Publication number: 20020134662Abstract: A process for separating a formaldehyde-containing product from a formalin solution comprising formaldehyde, water and methanol, wherein said formaldehyde-containing product contains substantially less water than said formalin solution, comprising distilling said formalin solution in the presence of a water entraining compound, especially methyl propionate or methyl methacrylate. The formaldehyde-containing product is suitable for use in a further process which requires a source of formaldehyde containing a relatively low level of water. One example of such a process is the reaction of methyl propionate with formaldehyde and methanol over a catalyst to produce methyl methacrylate.Type: ApplicationFiled: May 23, 2002Publication date: September 26, 2002Applicant: Ineos Acrylics UK Ltd.,Inventor: William David Parten
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Patent number: 6455732Abstract: Pure acrylic acid is stored and/or transported by a process in which the pure acrylic acid is stored and/or transported as liquid aqueous solution at ≦15° C.Type: GrantFiled: April 21, 2000Date of Patent: September 24, 2002Assignee: BASF AktiengesellschaftInventors: Heinrich Aichinger, Klaus Joachim Müller-Engel, Gerhard Nestler, Jürgen Schröder
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Patent number: 6448439Abstract: A process for preparing acrylic acid or methacrylic acid comprises preparing a gaseous product mixture having essentially the composition of a reaction mixture of the catalytic gas phase oxidation of C3-/C4-alkanes, -alkenes, -alkanols and/or -alkanals and/or precursors thereof to form acrylic acid or methacrylic acid. The product is removed from the gaseous product mixture by a process comprising the following steps: (a) condensing said gaseous product mixture, (b) crystallizing acrylic acid or methacrylic acid from the solution obtained in step (a), (c) removing the resulting crystals from the mother liquor, and (d) recycling at least a portion of said mother liquor from step (c) into step (a).Type: GrantFiled: March 13, 2000Date of Patent: September 10, 2002Assignee: BASFAktiengesellschaftInventors: Bernd Eck, Otto Machhammer, Theo Proll, Volker Schliephake, Joachim Thiel, Klaus Bröllos
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Patent number: 6441228Abstract: The present invention provides an apparatus for producing (meth)acrylic acid and a process for producing (meth)acrylic acid with this apparatus wherein the apparatus enables to produce (meth)acrylic acid stably for a long period of time by effectively inhibiting the polymerization of (meth)acrylic acid in its production process (for example, in a reboiler). At least a part of the apparatus is made of a nickel-chromium-iron alloy with a molybdenum content of 3 to 20 mass %, but not including 3 mass %, or with a molybdenum content of 1 to 4 mass % and a copper content of 0.5 to 7 mass %.Type: GrantFiled: December 12, 2000Date of Patent: August 27, 2002Assignee: Nippon Shokubai Co., Ltd.Inventors: Sei Nakahara, Kazuhiko Sakamoto, Yukihiro Matsumoto, Kenji Sanada, Masatoshi Ueoka
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Patent number: 6436245Abstract: A purification tower for purifying liquid by contacting the liquid with gas, the purification tower including: (a) a shell; and (b) a plurality of baffles, each of which is fixed to an internal surface of the shell, (i) said each baffle having a flat upper surface and a plurality of openings are formed in each of the baffle so that the liquid and the gas pass through the openings; (ii) any adjacent pair of the baffles are arranged so that a bottom of the shell is covered by the pair of the baffles viewing in an longitudinal direction of the shell. The present invention thus configured can provide a process and an apparatus for the purification of even an organic compound containing a readily-blocking substances, which are capable of continuously purifying such an organic substance over the long time without discontinuing operations.Type: GrantFiled: June 2, 2000Date of Patent: August 20, 2002Assignee: Nippon Shokubai Co., Ltd.Inventors: Takeshi Nishimura, Yukihiro Matsumoto
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Patent number: 6433222Abstract: A process for the preparation of acrylic acid by: (a) preparation of a gaseous product mixture which essentially has the composition of a reaction mixture of catalytic gas-phase oxidation of C3-alkanes, C3-alkenes, C3-alkanols and/or C3-alkanals and/or intermediates thereof to acrylic acid, which comprises (b) condensation of the gaseous product mixture, (c) crystallization of the acrylic acid from the solution obtained in stage (b), with partial evaporation of the solution under reduced pressure, (d) isolation of the resulting crystals from the mother liquor, (e) recycling of at least a part of the mother liquor from stage (d) to stage (b) and (f) recycling of at least a part of the evaporated solution from stage (c) to stage (b).Type: GrantFiled: January 22, 2001Date of Patent: August 13, 2002Assignee: BASF AktiengesellschaftInventors: Bernd Eck, Jörg Heilek, Volker Schliephake, Theo Proll, Klaus Bröllos, Otto Machhammer, Joachim Thiel
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Patent number: 6433163Abstract: The present invention provides a novel process for the removal and recovery of penicillin and organic acids from process streams and waste waters. The process of the present invention utilizes a combination of a supported liquid membrane (SLM) and a strip dispersion to improve extraction of the penicillin and organic acids while increasing membrane stability and reducing processing costs.Type: GrantFiled: April 3, 2000Date of Patent: August 13, 2002Assignee: Commodore Separation Technoligies, Inc.Inventor: W. S. Winston Ho
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Patent number: 6426433Abstract: In a process for the preparation of acrolein and/or acrylic acid from propane, the propane is subjected, in a first reaction stage, to a partial oxydehydrogenation with molecular oxygen under homogeneous and/or heterogeneous catalysis to give propene and the product gas mixture formed in the first reaction stage is then used for the preparation of acrolein and/or acrylic acid by gas-phase catalytic propene oxidation.Type: GrantFiled: February 20, 2001Date of Patent: July 30, 2002Assignee: BASF AktiengesellschaftInventors: Otto Machhammer, Andreas Tenten, Harald Jachow, Susanne Haupt, Heiko Arnold, Signe Unverricht
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Publication number: 20020087029Abstract: In a process for purifying acrylic acid by crystallization by means of vacuum evaporation, a solution which contains acrylic acid and water and may contain further components is crystallized by means of vacuum evaporation with formation of a liquid phase, consisting of a mother liquor containing more than 10% by weight of water and of the crystals, and a vapor phase, the vapor phase is introduced into a liquid material in a condensation zone with formation of a liquid condensation mixture, and the liquid condensation mixture is recycled at least partly to the condensation zone, the operating conditions in the condensation zone being established so that no solid is precipitated.Type: ApplicationFiled: July 21, 1999Publication date: July 4, 2002Inventors: BERND ECK, JORG HEILEK, VOLKER SCHLIEPHAKE
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Patent number: 6414183Abstract: The present invention provides a method for stabilizing waste oil which is taken of each chemical apparatus of the manufacturing line of (meth)acryl acid and/or ester thereof, and treating the waste oil such as draining it out of the production apparatus, for example, a distillation tower from its bottom, sending and transporting it by a pump through a pipeline, and storing it in a storage tank in a simple manner while keeping the waste oil in a stable state. The waste oil can be stabilized by coexisting with solvent. The solvent used in the present invention is typically at least one selected from the group consisting of water, alcohol, ether, carboxylic acid, ketone, aromatic hydrocarbons, and aliphatic hydrocarbons.Type: GrantFiled: April 5, 2000Date of Patent: July 2, 2002Assignee: Nippon Shokubai Co., Ltd.Inventors: Kazuhiko Sakamoto, Sei Nakahara, Masatoshi Ueoka
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Patent number: 6414190Abstract: In a process for purifying acrylic acid by crystallization by means of vacuum evaporation, a solution which contains acrylic acid and water and may contain further components is crystallized by means of vacuum evaporation with formation of a liquid phase, consisting of a mother liquor containing more than 10% by weight of water and of the crystals, and a vapor phase, the vapor phase is introduced into a liquid material in a condensation zone with formation of a liquid condensation mixture, and the liquid condensation mixture is recycled at least partly to the condensation zone, the operating conditions in the condensation zone being established so that no solid is precipitated.Type: GrantFiled: July 21, 1999Date of Patent: July 2, 2002Assignee: BASF AktiengesellschaftInventors: Bernd Eck, Jörg Heilek, Volker Schliephake
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Patent number: 6413379Abstract: A process for the continuous recovery of (meth)acrylic acid from a liquid starting mixture containing (meth)acrylic acid, a high-boiling organic solvent and low boilers, medium boilers and high boilers is proposed, the mixture being separated into a first part-stream (a), which, in addition to (meth)acrylic acid, contains the low boilers and a part each of the medium boilers and high boilers, and a second part-stream (b), which contains the predominant part of the (meth)acrylic acid and is completely or virtually completely free of low boilers, and the (meth)acrylic acid being recovered from the part-stream (b).Type: GrantFiled: July 29, 1999Date of Patent: July 2, 2002Assignee: BASF AktiengesellschaftInventors: Otto Machhammer, Susanne Haupt, Volker Schliephake, Jürgen Schröder
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Patent number: 6409886Abstract: In distillation of easily polymerizable compounds such as (meth)acrylic acid and (meth)acrylic esters using a distillation unit, a liquid having substantially the same composition with that of a liquid surrounding a constitutive member placed in the distillation unit is sprayed by a spraying and supplying device. The liquid supplied by the spraying and supplying device preferably has a wetting liquid rate (of the sprayed and supplied liquid, a flow rate of a liquid attaching to and wetting the constitutive member) of 0.5 m3/m2hr or more relative to the surface area of the constitutive member. The liquid supplied by the spraying and supplying device preferably contains a polymerization inhibitor. It is also preferred to supply a gas containing molecular oxygen to the distillation unit. This process can effectively inhibit the polymerization of the easily polymerizable compounds, which polymerization is liable to occur inside the distillation unit.Type: GrantFiled: April 14, 2000Date of Patent: June 25, 2002Assignee: Nippon Shokubai Co., Ltd.Inventors: Yukihiro Matsumoto, Takeshi Nishimura
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Patent number: 6407287Abstract: In a method for producing acrylic acid by the steps of a reaction of catalytic gas phase oxidation, absorbing the acrylic acid with an absorbent, and dehydrating the acrylic acid-containing aqueous solution, the method is characterized that the step of dehydration comprises adding and an azeotropic solvent, distilling the resultant mixture, and adjusting the acrylic acid concentration at the top of the column in the range of 0.06-0.80 wt. %, thereby preventing the bottoms of the azeotropic dehydration column from substantially containing the azeotropic solvent and water. As results, the acrylic acid is kept from forming a polymer in any of the distillation columns involved in the production, and effective utilization of acrylic acid.Type: GrantFiled: March 7, 2001Date of Patent: June 18, 2002Assignee: Nippon Shokubai Co., Ltd.Inventors: Yukihiro Matsumoto, Takeshi Nishimura, Kazuhiko Sakamoto, Hidefumi Haramaki
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Patent number: 6399817Abstract: This invention relates to a process for preparing acrylic acid which utilizes an aqueous stream which includes recycled wastewater, at least part of which is stripped of undesirable components in a stripping column prior to being recycled to an acrylic acid absorber.Type: GrantFiled: March 1, 2000Date of Patent: June 4, 2002Assignee: Rohm and Haas CompanyInventors: Josefina Tseng Chapman, James Clarence Day, Donald Alan Ebert, Thomas Albert Kaminski, Robert Michael Mason, Chorng-Shyuan Tsay
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Patent number: 6395140Abstract: In a process for the preparation of (meth)acrylic acid from a mixture which contains (meth)acrylic acid and a solvent having a boiling point above the boiling point of (meth)acrylic acid by distillation of the mixture in a column which is connected to an evaporator and has a stripping section and a rectifying section, between which the mixture is fed in, and a side take-off for the (meth)acrylic acid, a polymeization inhibitor is fed into the column in the region of the top of the column and in the region of the side take-off, that amount of polymerization inhibitor which is introduced in the region of the top of the column being smaller than the amount introduced in the region of the side take-off.Type: GrantFiled: April 24, 2000Date of Patent: May 28, 2002Assignee: BASF AktiengesellschaftInventors: Holger Herbst, Gerhard Nestler, Ulrich Hammon
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Patent number: 6388129Abstract: In a process for the preparation of acrolein and/or acrylic acid from propane, the propane is subjected, in a first reaction stage, to a partial oxydehydrogenation with molecular oxygen under homogeneous and/or heterogeneous catalysis to give propene and the product gas mixture formed in the first reaction stage is then used for the preparation of acrolein and/or acrylic acid by gas-phase catalytic propene oxidation.Type: GrantFiled: February 20, 2001Date of Patent: May 14, 2002Assignee: BASF AktiengesellschaftInventors: Otto Machhammer, Andreas Tenten, Harald Jachow, Susanne Haupt, Heiko Arnold, Signe Unverricht
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Patent number: 6380427Abstract: A process for purification of (meth)acrylic acid which comprises adding to a crude (meth)acrylic acid one or two or more polar organic substances as a second component at a concentration of 1-35% by weight, crystallizing (meth)acrylic acid from the resulting (meth)acrylic acid solution, and separating the precipitated crystal of (meth)acrylic acid and a mother liquor from each other.Type: GrantFiled: January 28, 2000Date of Patent: April 30, 2002Assignee: Mitsubishi Rayon Co., Ltd.Inventors: Seiji Miyazaki, Akira Ogawa, Yasutaka Nakashima, Yoshiaki Kobayashi, Mikiyoshi Araki