Before Crystal Formation Patents (Class 585/817)
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Patent number: 8575412Abstract: Processes are provided for producing triphenylene by combining at least dodecahydrotriphenylene, a dehydrogenation catalyst such as palladium on carbon, and an aliphatic solvent having a boiling point greater than 180° C. to form a reaction mixture, heating the reaction mixture to at least about 180° C. but lower than the boiling point of the aliphatic solvent, maintaining the temperature of the reaction mixture at 180° C. but lower than the boiling point of the aliphatic solvent, and passing a purge fluid comprising an inert fluid through the reaction mixture, for a period of time adequate for production of triphenylene.Type: GrantFiled: October 28, 2009Date of Patent: November 5, 2013Assignee: Albemarle CorporationInventors: Kevin Coppola, Christopher D. Claeboe, Bruce C. Berris
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Patent number: 8558048Abstract: This invention relates to methods for the stabilization, storage and delivery of biologically active macromolecules, such as proteins, peptides and nucleic acids. In particular, this invention relates to protein or nucleic acid crystals, formulations and compositions comprising them. Methods are provided for the crystallization of proteins and nucleic acids and for the preparation of stabilized protein or nucleic acid crystals for use in dry or slurry formulations. The present invention is further directed to encapsulating proteins, glycoproteins, enzymes, antibodies, hormones and peptide crystals or crystal formulations into compositions for biological delivery to humans and animals. According to this invention, protein crystals or crystal formulations are encapsulated within a matrix comprising a polymeric carrier to form a composition.Type: GrantFiled: October 30, 2009Date of Patent: October 15, 2013Assignee: Althea Technologies, Inc.Inventors: Alexey L. Margolin, Nazar K. Khalaf, Nancy L. St. Clair, Scott L. Rakestraw, Bhami C. Shenoy
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Patent number: 8163970Abstract: A method including carrying out adiabatic cooling and evaporation operation of a coolant in a crystallizer (20) for a mixture solution of a target organic compound containing the coolant; taking out crystal slurry produced by the operation from the crystallizer (20); pressurizing evaporated vapor to a pressure higher than the operation pressure in the crystallizer (20) by a compressor (30) and then introducing the vapor to an absorption condenser (10); cooling for condensation the mixture solution of organic compound and the evaporated vapor that has been pressurized while allowing them to contact each other in the absorption condenser (10); introducing the crystal slurry taken out of the crystallizer (20) to a purification means (70) for purification of the crystal; and introducing a clarified liquid in the purification means (70) to at least one of the crystallizer (20) and the absorption condenser (10).Type: GrantFiled: March 7, 2006Date of Patent: April 24, 2012Assignee: Tsukishima Kikai Co., Ltd.Inventors: Keizo Takegami, Junji Wakayama, Kiwamu Ishii, Kenji Ouchi
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Publication number: 20100228070Abstract: The present invention relates to a method for achieving high purity separation and refinement by controlling morphology and particle size of 2,6-dimethylnaphthalene. And more particularly, the present invention relates to a method for obtaining high purity 2,6-dimethylnaphthalene crystals, in which crystallization is carried out with a solvent that enables the crystals to form a square-platy shape. During the process, crystallization variables such as, stirring speed, cooling speed, solvent and composition ratio, are adjusted to control morphology and particle size of 2,6-dimethylnaphthalene and to remove aggregation, thereby obtaining 2,6-dimethylnaphthalene crystals of high purity.Type: ApplicationFiled: September 25, 2008Publication date: September 9, 2010Applicant: HYOSUNG CORPORATIONInventors: Yang-Ho Cheon, Young-Gyo Choi
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Patent number: 7605296Abstract: A method for separating and purifying 2,6-dimethylnaphthalene, is provided in which 2,6-dimethylnaphthalene of high purity is obtained from a mixture of dimethylnaphthalene isomers with a high yield, by means of a combined process of column melt crystallization and sweating operation.Type: GrantFiled: November 8, 2006Date of Patent: October 20, 2009Assignee: Hyosung CorporationInventors: Yang-Ho Chenon, Young-Gyo Choi
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Patent number: 6894202Abstract: An object of the present invention is to provide a method for manufacturing 2,6-DMN, in which even when a mixture containing DMN isomers which includes 5 wt % or more of 2,7-DMN is used, a highly pure 2,6-DMN can be obtained. The method for manufacturing the highly pure 2,6-dimethylnaphthalene of the present invention comprises performing cooling crystallization of a mixture containing dimethylnaphthalenes which includes 2,6-dimethylnaphthalene, performing solid-liquid separation to obtain a solid component, and washing the solid component using a solvent, wherein the solid-liquid separation performed after the cooling crystallization includes press filtration.Type: GrantFiled: August 30, 2000Date of Patent: May 17, 2005Assignee: Kobe Steel, Ltd.Inventors: Koji Yamamoto, Seiichi Yamamoto, Takeharu Tanaka, Masahiro Motoyuki, Shingo Yoshida
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Patent number: 6737558Abstract: Process for the separation of 2,6-dimethylnaphthalene from mixtures containing it, comprising the following operations: crystallization by the addition of a solvent and cooling of the mixture to a temperature higher than the formation value of the first eutectic; removal of the mother liquor by repeated washings; dissolution of the solid obtained; crystallization by cooling; filtration.Type: GrantFiled: May 9, 2001Date of Patent: May 18, 2004Assignees: ENICHEM S.p.A., ENI S.p.A.Inventors: Renzo Bignazzi, Gianni Pandolfi
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Patent number: 6525235Abstract: The present invention provides a method for manufacturing a highly pure 2,6-dimethylnaphthalene having a purity of 99% or more even when a mixture of dimethylnaphthalene isomers containing 5 wt % or more of 2,7-dimethylnaphthalate is used as a feedstock. The method for manufacturing 2,6-dimethylnaphthalene comprises a step of performing crystallization and solid-liquid separation of a liquid primarily containing dimethylnaphthalene isomers so that the liquid is separated into a cake containing the dimethylnaphthalene isomers and a mother liquor, and a step of performing separation/purification of the cake. In the method described above, the crystallization and the solid-liquid separation are performed under the condition in which the ratio of the content of 2,6-dimethylnaphthalene in the mother liquor to that of 2,7-dimethylnaphthalene therein is not less than 1 so that the content of 2,6-dimethylnaphthalene in the cake is 60% or more and that the content of 2,7-dimethylnaphthalene therein is 6.5% or less.Type: GrantFiled: October 1, 2001Date of Patent: February 25, 2003Assignee: Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.)Inventors: Shingo Yoshida, Masahiro Motoyuki, Tomoki Uemura, Koji Yamamoto
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Publication number: 20020023318Abstract: Process for the separation of 2,6-dimethylnaphthalene from mixtures containing it, comprising the following operations:Type: ApplicationFiled: May 9, 2001Publication date: February 28, 2002Applicant: ENICHEM S.p.A.Inventors: Renzo Bignazzi, Gianni Pandolfi
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Patent number: 6291735Abstract: A process is provided for the preparation of high-purity indene. According to the process, impurities are eliminated by crystallization from an indene stock which is available in a concentrated form by distillation of a coal tar fraction and/or a petroleum fraction. High-purity indene having a purity of 99 wt. % or higher can be obtained.Type: GrantFiled: September 17, 1999Date of Patent: September 18, 2001Assignee: ADCHEMCO CorporationInventors: Yasuyuki Takigawa, Hiromi Nakaoka
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Patent number: 6072098Abstract: There are disclosed an industrially advantageous process for efficiently producing highly pure 2,6-dimethylnaphthalene (DMN) in high yield from a mixture of DMN by carrying out in turn, the steps of isomerizing a mixture of DMN in the presence of a catalyst; crystallizing the isomerization reaction product in the presence of a solvent (e.g.Type: GrantFiled: December 30, 1996Date of Patent: June 6, 2000Assignee: Mitsubishi Gas Chemical Company, Inc.Inventors: Makoto Takagawa, Ryusuke Shigematsu
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Patent number: 5948949Abstract: A process for producing highly pure 2,6-dimethylnaphthalene in a high yield from a mixture of dimethylnaphthalene isomers in the presence of a solvent, such as an aliphatic or alicyclic saturated hydrocarbon. Highly pure 2,6-dimethylnaphthalene can be produced steadily for a long time by filtering the 2,6-dimethylnaphthalene crystal precipitated by the crystallizing by using a filtration apparatus, such as a rotary vacuum filter, peeling-off the filtered cake from a filter cloth and cleaning the filter cloth with a solvent, at a temperature not lower than a filtration temperature.Type: GrantFiled: December 30, 1996Date of Patent: September 7, 1999Assignee: Mitsubishi Gas Chemical Company, Inc.Inventors: Makoto Takagawa, Ryusuke Shigematsu, Kuniaki Ageishi, Ko Kedo
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Patent number: 5264653Abstract: A process for purifying 1,1,3,4,4,6-hexamethyltetralin is disclosed comprising melting crude 1,1,3,4,4,6-hexamethyltetralin in methanol with heating, cooling the resulting suspension, and adding seed crystals at a temperature of 45.degree.-60.degree. C.; as well as a process for purifying 1,1,3,4,4,6-hexamethyltetralin comprising recrystallizing crude 1,1,3,4,4,6-hexamethyltetralin from a mixed solvent of methanol and a solvent capable of easily dissolving 1,1,3,4,4,6-hexamethyltetralin, the proportion of this solvent being 10 to 25% by weight based on the weight of methanol. These processes make it possible to obtain 1,1,3,4,4,6-hexamethyltetralin of high purity easily with high recovery by purifying crude 1,1,3,4,4,6-hexamethyltetralin.Type: GrantFiled: September 30, 1992Date of Patent: November 23, 1993Assignee: Sumitomo Chemical Company, LimitedInventors: Nobuaki Tabei, Hiroshi Sato
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Patent number: 4992619Abstract: The invention intends to separating a methyl derivative of naphthalene (2,6-dimethyl naphthalene or 2-methyl naphthalene) from a mixture material in a high purity more than 98 weight %. The starting material is preliminarily treated at a raised temperature up to 220.degree. c. at the highest and with LHSV of 0.1-6 Hr.sup.-1 in the presence of an acid catalyst usually used for olefin polymerization. The treated material is distillated to remove the polymerized impurities and to raise the naphthalene derivative content at least up to 50 weight %. And then the obtained material is subjected to the crystallization under a pressure of 500-2500 kgf/cm.sup.2 at a temperature of 80.degree.-150.degree. C. (for 2,6-DMN) or 10.degree.-35.degree. C. (for 2-MN).Type: GrantFiled: March 7, 1989Date of Patent: February 12, 1991Assignees: Showa Shell Sekiyu K.K., Kobe Steel Ltd.Inventors: Shunichi Koide, Shinji Aihara, Hiroshi Takeshita, Harumasa Tanabe, Masami Takao, Hitoshi Hatakeyama
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Patent number: 4956520Abstract: Separation of a crystallizable component, especially paraxylene, from solution by chilling to form a slurry of crystals and liquid, separating crystals of the component in a first separator while simultaneously washing the crystals with a wash liquid and then re-melting the crystals, re-chilling them, separating the crystals in a second separator and washing them with a second wash liquid.Type: GrantFiled: October 9, 1987Date of Patent: September 11, 1990Assignee: Imperial Chemical Industries PLCInventors: David S. Flett, John E. Lloyd
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Patent number: 4952750Abstract: This process is an improvement of a process described in German Open Patent Application No. 3703646 for obtaining a p-xylene product with a purity of at least 99.5%. The inert fluid used as a cold carrier is mixed with a crude product starting material, which has a high p-xylene content, in a mixing vessel under rotation to form a resultant mixture. Subsequently the resultant mixture is concentrated to a crystal content of from 30% to 70% and after that the p-xylene crystals are separated in a separator. The purity of the product p-xylene can be increased by heating these crystals in the separator.Type: GrantFiled: April 14, 1989Date of Patent: August 28, 1990Assignee: Krupp Koppers GmbHInventor: Guenter Puppel
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Patent number: 4915794Abstract: This invention relates to a process for producing an olefin product having an enhanced alpha olefin content from an olefin feedstock containing internal olefins or a mixture of internal and alpha olefins which includes:(a) contacting the feedstock with an anthracene and a double-bond isomerization catalyst at a temperature ranging from about 150.degree. to about 275.degree. C. to form an olefin adduct with anthracene,(b) separating the adduct from the product of step (a),(c) heating the separated adduct at a temperature ranging from about 250.degree. to about 400.degree. C. to produce anthracene and an olefin product enhanced in alpha olefin content over the alpha olefin content of the feedstock, and(d) separating anthracene from the product of step (c) to produce the product enhanced in alpha olefin.Linear olefins are a preferred feedstock.Type: GrantFiled: October 27, 1988Date of Patent: April 10, 1990Assignee: Shell Oil CompanyInventors: Lynn H. Slaugh, Howard L. Fong
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Patent number: 4914257Abstract: The method for separating from a mother liquor containing at least two liquids, one of the two liquids including the steps of:(a) forming a precipitatable complex from one of the liquids and a complexing agent;(b) precipitating the precipitatable complex from the method liquor; and(c) recovering the second liquid from the remaining mother liquor. Typically, the two liquid substances are tetrahydrofuran and toluene and the complexing agent is titanium tetrachloride. The precipitatable complex is TiCl.sub.4.2C.sub.4 H.sub.8 O or TiCl.sub.4.C.sub.4 H.sub.8 O. Preferably, a cooling step is included in the method to enhance the removal of the precipitatabe complex. Superfractionation of the remaining liquor in distillation columns enables one to recover toluene, hexane, titanium tetrachloride and tetrahydrofuran. An apparatus for carrying out the method of recovering solvents in also disclosed.Type: GrantFiled: May 23, 1988Date of Patent: April 3, 1990Assignee: Amoco CorporationInventors: Steven A. Cohen, James H. Lee, David B. Manley
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Patent number: 4902850Abstract: A method of purification for anethole which involves forming an aqueous emulsion of crude anethole and crystallizing anethole from the emulsion. The process provides a purified anethole having improved odor and taste.Type: GrantFiled: August 5, 1988Date of Patent: February 20, 1990Assignee: Arizona Chemical CompanyInventor: Curry B. Davis
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Patent number: 4900717Abstract: In a process for selective crystallization of 2,6-dialkyl-naphthalene selected from the group consisting of methyl-n-propyl-naphthalene, methyl isopropyl-naphthalene, ethyl-isopropyl-napthalene, ethyl-n-butyl-naphthalene, di-n-propyl-naphthalene, diisopropyl-naphthalene, methyl-amyl-naphthalene, ethyl-amyl-naphthalene, propyl-amyl-naphthalene, di-n-butyl-naphthalene and diisobutyl-naphthalene from their isomer mixtures from a polar solvent solution, the improvement comprising effecting the crystallization with constant stirring at a temperature from 25.degree. to -30.degree. C. to obtain the 2,6-dialkyl-naphthalene at least 95% pure.Type: GrantFiled: February 4, 1988Date of Patent: February 13, 1990Assignee: Rutgerswerke AGInventors: Wilhelm Holtmann, Robert Zellerhoff, Rudolf Oberkobusch, Peter Staglich, Bernhard Charpey
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Patent number: 4331826Abstract: A process and an apparatus therefor are described for separating p-xylene from a p-xylene containing hydrocarbon liquid feed material by crystallization, said process comprising (1) mixing a p-xylene containing hydrocarbon feed material with an inert liquid refrigerant, (2) feeding the mixed liquid into a lower part of a bubble tower type crystallization tower as an ascending current, (3) evaporating the refrigerant by the lowering of the liquid static pressure caused by ascent of the mixed liquid and by the transfer of heat into the refrigerant due to solidification of p-xylene and by the lowering of the temperature of the mixed liquid, cooling the ascending liquid to form a slurry of p-xylene crystals in the hydrocarbon liquid, (4) separating the inert refrigerant as a vapor from the liquid surface of the upper part of the crystallization zone, and (5) separating p-xylene crystals from the slurry discharged from the upper part of the crystallization zone.Type: GrantFiled: March 16, 1981Date of Patent: May 25, 1982Assignee: Kawasaki Jukogyo Kabushiki KaishaInventor: Saburo Kagawa
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Patent number: 4153630Abstract: An inclusion compound comprising meta-cyclophane of the formula ##STR1## and at least one benzene derivative included therein. And a process for separating an isomer containing a substituent at least at the 1- and 4-positions from a mixture containing isomers of a benzene derivative, which comprises contacting the meta-cyclophane with the mixture containing isomers of a benzene derivative thereby to form an inclusion compound in which an isomer containing a substituent at least at the 1- and 4-positions is included in the meta-cyclophane, then separating the inclusion compound from the mixture, and thereafter separating the isomer from the inclusion compound.Type: GrantFiled: October 26, 1976Date of Patent: May 8, 1979Assignee: Teijin LimitedInventors: Yataro Ichikawa, Yoshiyuki Yamanaka, Hideki Tsuruta, Mamoru Yamamoto, Kenichi Kato