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公开(公告)号：DE69313595T2
公开(公告)日：1998-04-02
申请号：DE69313595
申请日：1993-12-08
Applicant: DAICEL CHEM , NIPPON PETROCHEMICALS CO LTD
Inventor： OHYAMA KYUICHI , TOKUMOTO YUICHI , SHIMADA GIICHI , SAKAMOTO KAZUO
Abstract: Disclosed is an improved process for the refinement of isopropyl acetate, whereby there can be effectively prepared isopropyl acetate having a high purity of, for example, approximately 99.9%, in which a distillate fraction having a carbon number of 3 obtained by catalytically cracking petroleums such as naphtha or a crude propylene by-produced in a process for the preparation of isobutene by the dehydrogenation of isobutane.
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公开(公告)号：DE69313595D1
公开(公告)日：1997-10-09
申请号：DE69313595
申请日：1993-12-08
Applicant: DAICEL CHEM , NIPPON PETROCHEMICALS CO LTD
Inventor： OHYAMA KYUICHI , TOKUMOTO YUICHI , SHIMADA GIICHI , SAKAMOTO KAZUO
Abstract: Disclosed is an improved process for the refinement of isopropyl acetate, whereby there can be effectively prepared isopropyl acetate having a high purity of, for example, approximately 99.9%, in which a distillate fraction having a carbon number of 3 obtained by catalytically cracking petroleums such as naphtha or a crude propylene by-produced in a process for the preparation of isobutene by the dehydrogenation of isobutane.
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公开(公告)号：EP0987261A4
公开(公告)日：2003-02-05
申请号：EP99905217
申请日：1999-02-17
Applicant: DAICEL CHEM
Inventor： TANAKA YASUTAKA , UENAKAI HIROAKI , SHIMADA GIICHI
IPC: C07D317/26 , C07D317/22
CPC classification number: C07D317/26
Abstract: A process for producing a dialdehyde monoacetal (III) from a dialdehyde (I) and a diol (II), characterized by reacting the dialdehyde (I) with twice or more, on the molar basis, as much the diol (III) to give a dialdehyde bisacetal (IV) and then reacting this dialdehyde bisacetal (IV) with a dialdehyde (III); and a process for producing glutaraldehyde monoacetal by reacting 2-Y-3,4-dihydro-2H-pyran with a diol, characterized by reacting in the second step glutaraldehyde (iv) formed as a by-product with glutaraldehyde bisacetal (v) formed as another by-product to give glutaraldehyde monoacetal (iii).
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公开(公告)号：JP2000038384A
公开(公告)日：2000-02-08
申请号：JP22371398
申请日：1998-07-23
Applicant: DAICEL CHEM
Inventor： TANAKA YASUTAKA , SHIMADA GIICHI
IPC: C07D317/26 , C07D319/06 , C07D321/00 , C07D321/06 , C07D321/12
Abstract: PROBLEM TO BE SOLVED: To obtain the subject monoacetal compound in a high yield by specifying an initial distillation temperature on isolating glutaraldehyde monoacetal by a distillation from a crude reaction liquid obtained after reacting dihydropyranes with a diol. SOLUTION: This glutaraldehyde monoacetal of formula II is obtained by reacting 2-Y-3, 4-dihydro-2H-pyrane of formula I (Y is hydroxy, an alkoxy or the like) or its nuclear-substituted derivative with a diol of the formula: HOROH [R is a 1-10C (un) saturated hydrocarbon], (suitably ethylene glycol or 1, 2-propylene glycol). In isolating the compound of the formula II after the reaction, an initial distillation operation for removing a low boiling component from the crude reaction liquid, is conducted while maintaining the temperature of the distillation bottom liquid at 100-200 deg.C, preferably at 130-180 deg.C. The reaction of the compound of the formula I with the diol, is preferably performed by using a sulfonic acid type cation exchange resin as a catalyst at 30-150 deg.C. The distillation of the crude reaction liquid is preferably performed after the removal of the catalyst.
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公开(公告)号：JPH01180844A
公开(公告)日：1989-07-18
申请号：JP399788
申请日：1988-01-12
Applicant: DAICEL CHEM
Inventor： AOYAMA HIROSHI , SHIMADA GIICHI
Abstract: PURPOSE:To obtain purified diglycerol useful as an intermediate, etc., for emulsifying agents, anti-fogging agents, etc., by subjecting a distillation residue containing diglycerol formed in producing synthetic glycerol to saponification treatment with an organic or inorganic alkali and water and/or an alcohol and distilling the saponified residue. CONSTITUTION:A distillation residue (colored residue, obtained as a bottom residue of a column for removing high-boiling substances from glycerol and consisting of 50% glycerol, 25% diglycerol and 25% tri- and polyglycerol), formed in producing synthetic glycerol and containing the diglycerol is initially subjected to continuous flash evaporation to recover the glycerol. The bottom residue is then subjected to saponification treatment with an organic or inorganic alkali (especially preferably NaOH, KOH, etc.) and water and/or an alcohol and subsequently distilled to afford the aimed purified diglycerol. As esterified or etherified diglycerol is useful as organic synthetic chemicals, anti- fogging agents and humectants or a raw material for coating resins, polyurethanes, etc.
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Patent Agency Ranking
公开(公告)号：JPH04154762A
公开(公告)日：1992-05-27
申请号：JP27674090
申请日：1990-10-16
Applicant: DAICEL CHEM
Inventor： SHIMADA GIICHI
IPC: C07D211/74 , B01J27/02 , B01J27/06 , B01J27/08 , B01J27/10 , B01J27/16 , B01J27/24 , B01J27/25 , B01J31/02 , B01J31/04 , C07B61/00
Abstract: PURPOSE:To obtain the subject compound in high yield for a short time in one stage by reacting acetone with ammonia at a specific molar ratio in the presence of an acid catalyst or iron salt of an organic carboxylic acid. CONSTITUTION:Acetone or an acidic condensate thereof with acetone (e.g. mesityl oxide, diacetone alcohol or acetonin) and ammonia are reacted at (20:1) to (4:1) molar ratio in the presence of an acidic catalyst (e.g. Lewis acid or protonic acid) or iron salt of an organic carboxylic acid (e.g. acetic or lactic acid) in an amount of 0.001-0.1mol, preferably 0.005-0.05mol based on 1mol acetone used at 50-150 deg.C, preferably 50-100 deg.C temperature under 60-100 atm pressure for 2-8hr in one stage to afford 2,2,6,6-tetramethyl-4-oxopiperidine. The formation of by-products, especially such products, having a higher boiling point than that of the objective compound and disturbing purification thereof is extremely reduced according to the aforementioned method.
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公开(公告)号：JPH01180845A
公开(公告)日：1989-07-18
申请号：JP541288
申请日：1988-01-13
Applicant: DAICEL CHEM
Inventor： AOYAMA HIROSHI , SHIMADA GIICHI
Abstract: PURPOSE:To produce purified diglycerol useful as an intermediate, etc., for emulsifying agents, anti-fogging agents, defoaming agents, humectants, etc., by heat-treating a distillation residue, formed in producing synthetic glycerol and containing diglycerol, then distilling and purifying the heat-treated residue. CONSTITUTION:A distillation residue (colored residue, obtained as a bottom residue of a column for removing high-boiling substances from glycerol and having composition of 50% glycerol, 25% diglycerol and 25% tri- and polyglycerol), formed in producing synthetic glycerol and containing the diglycerol is initially subjected to continuous flash evaporation to recover the glycerol. The bottom residue is then heat-treated at 170-230 deg.C, preferably 190-210 deg.C for preferably 20-25hr and subsequently purified by flash distillation to afford the aimed high-purity diglycerol. An esterified or etherified diglycerol is useful as organic synthetic chemicals, anti-fogging agents and humectants or a raw material for coating resins, polyurethanes, polyesters, etc.
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公开(公告)号：JPS6165834A
公开(公告)日：1986-04-04
申请号：JP18783584
申请日：1984-09-07
Applicant: Daicel Chem Ind Ltd
Inventor： TAKAHASHI SHIGEO , SHIMADA GIICHI
Abstract: PURPOSE: To remove trace of impurity from 1,3-butylene glycol, and to obtain the odorless substance of cosmetic grade, by carrying out the continuous distillation of 1,3-butylene glycol under reduced pressure with a thin-film evaporator while adding water to the system.
CONSTITUTION: 1,3-Butylene glycol having a purity of ≥98% is purified by the continuous distillation in the presence of water under reduced pressure (using a combination of a distillation column having low pressure drop and a thin-film evaporator). The characteristic smell remaining slightly in the raw material can be completely eliminated by this process. The water added to the system is preferably pure water or distilled water, and its amount is 5W50pts.wt. per 100pts.wt. of the raw material. The water may be added to the raw material before distillation or to the system through separate line. The column bottom temperature of the distillation column is preferably ≤130°C (corresponding to 40mmHg pressure), and the reboiler is preferably the one having short retention time of the process side stream (e.g. spontaneously flowing thin-film evaporator).
COPYRIGHT: (C)1986,JPO&JapioAbstract translation: 目的：为了从1,3-丁二醇中除去痕量的杂质，得到无味的化妆品等级，通过在薄膜蒸发器中进行减压下连续蒸馏1,3-丁二醇，同时加入水 到系统。 构成：通过在减压下的水的存在下（使用具有低压降的蒸馏塔和薄膜蒸发器的组合）连续蒸馏来纯化纯度> = 98％的1,3-丁二醇。 通过该处理可以完全消除原料中稍微保留的特征气味。 添加到系统中的水优选为纯水或蒸馏水，其量为5-50pts.wt。 每100pts.wt 的原料。 水可以在蒸馏前加入到原料中，也可以通过单独的管线加入到系统中。 蒸馏塔的塔底温度优选<= 130℃（对应于40mmHg压力），再沸器优选为工艺侧流的停留时间短（例如自发流动的薄膜蒸发器）。
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公开(公告)号：JPH11228566A
公开(公告)日：1999-08-24
申请号：JP5000998
申请日：1998-02-17
Applicant: DAICEL CHEM
Inventor： TANAKA YASUTAKA , SHIMADA GIICHI
IPC: C07D317/26
Abstract: PROBLEM TO BE SOLVED: To efficiently obtain the subject compound that is useful as a synthetic intermediate for medicines and agricultural chemicals by reaction between a dialdehyde and a diol at a specific ratio followed by the reaction of the resultant dialdehyde bisacetal with the dialdehyde. SOLUTION: In the first step, (A) a dialdehyde of formula I (R is a hydrocarbon residual group), for example, glutaraldehyde or the like, is allowed to react with a double or more molar amount, based on the component (A), of a diol of the formula: HO-R -OH (R is a hydrocarbon residual group), for example, ethylene glycol preferably in the presence of an acid catalyst such as a cationic ion-exchange resin or the like, preferably at 30-150 deg.C to form (C) a dialdehyde bisacetal of formula II, for example, glutaraldehyde bisacetal. In the second step, the product (C) is allowed to react with anhydrous component A preferably in the presence of the same catalyst as in the first step at the same reaction temperature as in the first step to give the objective compound of formula III.
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公开(公告)号：JPH06340570A
公开(公告)日：1994-12-13
申请号：JP13177793
申请日：1993-06-02
Applicant: DAICEL CHEM
Inventor： TANAKA YASUTAKA , SHIMADA GIICHI
Abstract: PURPOSE:To effectively prevent acrolein from polymerizing in producing, etc., the acrolein useful as a raw material, etc., for producing organic compounds by the coexistence of a polymerization inhibitor and oxalic acid in an aqueous solution of the acrolein containing iron ions dissolved therein. CONSTITUTION:A reactional gas containing acrolein after carrying out the vapor-phase oxidation of propylene is cooled with a large amount of water and the produced acrolein is simultaneously absorbed in water to provide an aqueous solution of the acrolein containing iron ions dissolved therein. A polymerization inhibitor such as hydroquinone, hydroquinone monomethyl ether, benzoquinone, p-nitrosophenol, p-aminophenol, m-dinitrobenzene, phenothiazine or Methylene Blue and oxalic acid are then added to coexist in the aqueous solution. Thereby, the acrolein is effectively prevented from polymerizing in a process for producing the acrolein important as a raw material for producing methionine, acrylic acid derivatives and other organic compounds.
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