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61. 发明专利

JPH0449253A PRODUCTION OF 2,6-DIMETHYLNAPHTHALENE 失效
公开(公告)号：JPH0449253A
公开(公告)日：1992-02-18
申请号：JP15776490
申请日：1990-06-18
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , MASUYAMA TETSUO , NAKANISHI AKIO , ASAHI YOSHIO
IPC分类号： B01J20/18 , B01J29/06 , C07B61/00 , C07C5/27 , C07C7/12 , C07C15/24
摘要： PURPOSE:To obtain the subject substance by separating the 2,6-isomer from a stock oil mainly containing a dimethylnaphthalene (DMN) isomer mixture, subjecting the residual stock oil to isomerizing reaction, increasing the 2,6-isomer concentration, removing components other than the DMN from the reaction product and circulating most thereof to the first step. CONSTITUTION:2,6-Dimethylnaphthalene (2,6-DMN) is separated from a stock oil mainly containing a DMN isomer mixture according to a continuous separation method, etc., using column chromatography to isomerize the resultant stock oil at the reduced 2,6-DMN concentration in the presence of a solid acid catalyst (e.g. H-ZSM-5 type zeolite) at 20-500 deg.C. Thereby, the 2,6-DMN concentration is increased to a composition near the thermodynamic equilibrium concentration. Low- and high-boiling substances are removed from the isomerizing reaction product and the 1,2-DMN is removed as much as possible. The obtained product is then circulated to the first step. The high-purity 2,6-DMN of >=99% purity can be efficiently produced by the aforementioned method.

62. 发明专利

JPH03204870A PRODUCTION OF LACTONES 失效
公开(公告)号：JPH03204870A
公开(公告)日：1991-09-06
申请号：JP24634190
申请日：1990-09-18
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , MIYAZAWA CHIHIRO , TAKAHASHI KAZUNARI , KAMEO HIROSHI
IPC分类号： C07D307/33 , B01J31/28 , C07B61/00 , C07D305/12
摘要： PURPOSE:To obtain lactones in high yield and to stabilize catalytic activity by hydrogenating a dicarboxylic acid, anhydride and/or ester thereof in the presence of ruthenium-based catalyst. CONSTITUTION:A dicarboxylic acid, a dicarboxylic acid anhydride and/or a dicarboxylic ester is hydrogenated in the presence of a ruthenium based catalyst in a liquid phase at 50-250 deg.C under 0.1-100kg/cm G pressure to give the objective lactone. A ruthenium-based catalyst containing (A) ruthenium, (2) an organic phosphine and (3) a conjugated salt group of acid having pka smaller than 2 is used as the ruthenium-based catalyst. A catalytic solution prepared by removing the lactone from the hydrogenated reaction product is recycled for hydrogenation reaction. Concentration of free organic phosphine in a liquid phase in hydrogenation reaction zone is maintained preferably 0.01-0.1wt.%.

63. 发明专利

JPH02141412A PRODUCTION OF CATALYST CONSISTING OF VANADIUM-PHOSPHORUS TYPE CRYSTALLINE OXIDE OR CATALYST CONTAINING THIS OXIDE 失效
公开(公告)号：JPH02141412A
公开(公告)日：1990-05-30
申请号：JP27232788
申请日：1988-10-28
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , KAWAKAMI TETSUGO , SUWA HIDEO , MIYASAKA MOTOYUKI
IPC分类号： C07D307/60 , B01J27/18 , B01J27/198 , C01B25/37 , C07B61/00
摘要： PURPOSE:To obtain a V-P type crystalline oxide useful as a material for a catalyst for producing maleic anhydride by the vapor phase oxidation of >=4C hydrocarbons by allowing a tetravalent V compd. to react with a quinquevalent P compd. in the presence of a specified seed crystal. CONSTITUTION:A precursor for V-P type crystalline oxide obtd. by a reaction of a tetravalent V compd. (e.g., V2O5) with a quinquevalent P compd. (e.g., P2O5) in an aq. medium is pulverized to obtain seed crystals having principal X-rays diffraction peaks as described in the table A and

64. 发明专利

JPH01311057A PRODUCTION OF ACRYLONITRILE AND/OR METHACRYLONITRILE 失效
公开(公告)号：JPH01311057A
公开(公告)日：1989-12-15
申请号：JP13805088
申请日：1988-06-04
申请人： MITSUBISHI CHEM IND
发明人： HATANO MASAKATSU , OSHIMA KAZUNORI , OTAKE MASAYUKI , IHARA TATSUYA
IPC分类号： C07C255/08 , B01J23/44 , C07B61/00 , C07C67/00 , C07C253/00 , C07C253/26
摘要： PURPOSE:To obtain acrylonitrile and/or methacrylonitrile in high use efficiency of ammonia by reacting propylene or isobutylene with ammonia and oxygen or oxygen-containing gas in the presence of a specific catalyst in a gas phase. CONSTITUTION:Propylene and/or isobutylene is reacted with ammonia and oxygen or an oxygen-containing gas in the presence of an oxide catalyst at 350-520 deg.C in a gas phase to give the aimed substance. An oxide shown by the formula (A is Fe, Sn or U; B is Cu, Mo or W; a is 20; b is 0.5-5; c is 0.002-0.3; d is 4-100; e is 0-5; z is number of oxygens required for satisfying valence of each of the above-mentioned components) is used as the catalyst. The catalyst is directly used as it is or supported on silica, titania, zirconia, etc.

65. 发明专利

JPH01201016A PRODUCTION OF VANADIUM-PHOSPHORUS-BASED CRYSTALLINE OXIDE OR CATALYST CONTAINING SAME 失效
公开(公告)号：JPH01201016A
公开(公告)日：1989-08-14
申请号：JP8692988
申请日：1988-04-08
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , KAWAKAMI TETSUGO
IPC分类号： C07D307/60 , B01J27/198 , C01B25/37 , C01B25/42 , C07B61/00
摘要： PURPOSE:To provide the title production process so designed that a vanadium- phosphorus (V-P)-based crystalline oxide having specific main X-ray diffraction peaks produced by the organic medium technique is subjected to steam treatment to enhance the purity of said oxide and improve the reproducibility of the activity of the catalyst as a sintered form therefrom. CONSTITUTION:A V-P-based crystalline oxide (precursor oxide) having main X-ray diffraction peaks shown in the table, produced by the reaction in an organic solvent is subjected to steam treatment to enhanced the purity of the crystal. Although the process for said steam treatment is not specified, the treatment can normally be conducted as follows: (1) a mixture of said precursor oxide and water is heated to generate steam, or (2) said mixture is fed with steam. Thence, the precursor oxide thus steam-treated is dried. The resultant precursor oxide, as a catalyst, active component of catalyst, or precursor thereof, can be used for e.g., the production of maleic anhydride by gaseous phase oxidation of a >=4C hydrocarbon.

66. 发明专利

JPH01186864A PRODUCTION OF N-ALKYL-SUBSTITUTED LACTAM 失效
公开(公告)号：JPH01186864A
公开(公告)日：1989-07-26
申请号：JP1130488
申请日：1988-01-21
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , FUKUSHIMA ISAMU , FUJITA KOICHI
IPC分类号： C07D211/76 , C07D207/267
摘要： PURPOSE:To obtain the title high-purity substance in high yield and recycle the eliminated alcohol through a process for preparing a secondary amine, by reacting a lactone compound with secondary amines in the presence of water in a specific amount and subjecting the resultant reaction product to dealcoholizing decomposition at a specific temperature. CONSTITUTION:A lactone compound (e.g., gamma-butyrolactone) is reacted with a secondary amine in the presence of water in a molar amount of 3-5 times based on the lactone compound and the resultant reaction product is then subjected to dealcoholizing decomposition at 240-265 deg.C to afford the title substance (e.g., N-alkyl-substituted 2-pyrrolidone). The eliminated alcohol can be then separated and recycled through a process for preparing the secondary amine. The selectivity for the lactam is high in the above-mentioned method with a low lactone content in the product and the lactam having excellent color tone is obtained. Availability is improved by changing a primary amine with the secondary amine. Since the boiling point is high, safety problems can be improved.

67. 发明专利

JPH01186863A PRODUCTION OF N-ALKYL-SUBSTITUTED LACTAM 失效
公开(公告)号：JPH01186863A
公开(公告)日：1989-07-26
申请号：JP1130388
申请日：1988-01-21
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , FUKUSHIMA ISAMU , FUJITA KOICHI
IPC分类号： C07D211/76 , C07D207/267
摘要： PURPOSE:To obtain the title high-purity substance in high yield, by reacting a lactone compound with a tertiary amine or tertiary or quaternary ammonium compound in the presence of water and then subjecting the resultant reaction product to dealcoholization reaction at a specific temperature. CONSTITUTION:A lactone compound (e.g., gamma-butyrolactone) is reacted with a tertiary amine or tertiary or quaternary ammonium compound in the presence of water in an molar amount of 3-5times based on the lactone compound and the resultant reaction product is then subjected to dealcoholization reaction at 240-270 deg.C (preferably 250-265 deg.C) to afford the title compound (e.g., N-alkyl substituted-2-pyrrolidone). The eliminated alcohol obtained by the above- mentioned method can be recycled for use in a preparation process of the amine. The title substance is nontoxic and widely used as solvents having excellent heat resistance, various organic synthetic intermediates or for polymerizing highly functional resins, forming or processing films, etc.

68. 发明专利

JPS6327474A PRODUCTION OF LACTAM 失效
公开(公告)号：JPS6327474A
公开(公告)日：1988-02-05
申请号：JP16949386
申请日：1986-07-18
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , FUKUSHIMA ISAMU
IPC分类号： C07B61/00 , B01J31/26 , C07D201/08
摘要： PURPOSE:To obtain a lactam useful as a raw material for organic syntheses, stable polar solvent, etc., in high selectivity on an industrial scale at a low cost, by adding a small amount of an acidic substance to a reaction system and reducing a specific cyclic acid imide with hydrogen in the presence of a metallic catalyst. CONSTITUTION:The objective compound of formula IV can be produced by reducing a cyclic acid imide of formula I [R is H or 1-5C alkyl; R is >=2C saturated or unsaturated bivalent organic group) (e.g. N-methylsuccinimide) or its precursor such as the compound of formula III with H2 in the presence of a catalyst composed of at least one kind of metallic component selected from Co, Mo, W, etc., at 160-300 deg.C under 10-300kg/cm G pressure in a reaction system added with 10-5,000ppm of an acidic substance such as phosphoric acid, concentrated sulfuric acid, etc., based on the flow rate (weight) in the reaction system. EFFECT:By-production of gaseous component such as lower hydrocarbon (e.g. CH3) can be suppressed. USE:Raw material for the synthesis of polymers by ring-opening polymerization, etc.

69. 发明专利

JPS61183233A METHOD FOR SEPARATING 8C AROMATIC HYDROCARBON 失效
公开(公告)号：JPS61183233A
公开(公告)日：1986-08-15
申请号：JP2256685
申请日：1985-02-07
申请人： MITSUBISHI CHEM IND
发明人： OTAKE MASAYUKI , MORI TOMOYUKI , NAKANISHI AKIO
IPC分类号： C07C7/13 , C07C1/00 , C07C15/08 , C07C67/00
摘要： PURPOSE:To efficiently adsorb and separate a sepcific isomer from an 8C aromatic hydrocarbon isomer mixture, by using a specific dialkyl ketone as a desorption agent and further a zeolite based adsorbent having adsorption selectivity between the 8C aromatic hydrocarbon isomers. CONSTITUTION:A specific isomer, particularly p-xylene is adsorbed and separat ed from an 8C aromatic hydrocarbon isomer mixture, particularly the above- mentioned mixture containing three isomers of xylene using a zeolite based adsorbent having adsorption selectivity between the 8C aromatic hydrocarbon isomers. In the process, a dialkyl ketone having >=6 total carbon number such as methyl isobutyl ketone, diisopropyl ketone, isopropyl isobutyl ketone or/and diisobutyl ketone, particularly diisobutyl ketone as a desorption agent to improve the adsorption selectivity between the respective isomers and adjust the adsorp tion selectivity between the desorption agent and the isomer to be desorbed to nearly 1. Thus, the aimed isomer is sufficiently separated.

70. 发明专利

JPS6130545A Hydrogenation of unsaturated carbonyl compound 失效
标题翻译：不饱和碳化合物的氢化
公开(公告)号：JPS6130545A
公开(公告)日：1986-02-12
申请号：JP15021684
申请日：1984-07-19
申请人： Mitsubishi Chem Ind Ltd
发明人： OTAKE MASAYUKI , KOIKE YASUO
IPC分类号： C07C45/62 , B01J23/00 , B01J23/58 , C07B61/00 , C07C45/00 , C07C47/02 , C07C49/04 , C07C49/385 , C07C67/00
CPC分类号： Y02P20/52
摘要： PURPOSE: To produce the titled compound easily, in high purity, by the liqid- phase hydrogenation of an unsaturated carbonyl compound in the presence of a catalyst containing specific amounts of palladium and an alkali metal as active components of the catalyst.
CONSTITUTION: The objective compound is produced by the liquid-phase hydrogenation of an unsaturated carboxyl compound at 40W200°C under atmospheric pressure W50kg/cm
2 in the presence of a catalyst containing palladium and an alkali metal supported on a carrier and having alkali metal/palladium atomic ratio of 0.7W3.5, especially 1.0W2.0 determined by X-ray photo-electron spectrometry at the surface of the catayst. The catalyst can be prepared e.g. by supporting a soluble palladium salt, e.g. palladium chloride, etc. as a palladium component on a carrier, reducing the supported palladium compound to obtain a palladium-supported catalyst, and then applying an alkali metal salt, etc. as the alkali metal component from a solution to the palladium catalyst.
COPYRIGHT: (C)1986,JPO&Japio
摘要翻译：目的：通过在含有特定量的钯和作为催化剂的活性成分的碱金属的催化剂存在下，通过不饱和羰基化合物的液相氢化，容易地制备标题化合物。构成：目标化合物是通过不饱和羧基化合物在40-200℃，常压-50kg / cm 2下，在含钯和碱金属的催化剂存在下进行液相氢化生产的载体，其碱金属/钯原子比为0.7-3.5，特别是1.0-2.0，通过X射线光电子能谱法测定。催化剂可以例如制备。通过支持可溶性钯盐，例如氯化钯等作为载体上的钯组分，还原负载的钯化合物以获得钯负载的催化剂，然后将碱金属盐等作为碱金属成分从溶液中加入到钯催化剂中。

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