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1. 发明专利

JPH05208928A PRODUCTION OF CRESOLS 失效
公开(公告)号：JPH05208928A
公开(公告)日：1993-08-20
申请号：JP1613692
申请日：1992-01-31
申请人： SUMITOMO CHEMICAL CO
发明人： IKIMI KIYOSHI , IKEDA YOICHI , MURAKAMI AKIRA , OKAMOTO KAZUNARI , TOKUMARU TORU , HAZAMA YASUO
IPC分类号： B01J23/44 , B01J23/755 , B01J23/86 , B01J27/02 , B01J27/10 , B01J27/19 , B01J31/02 , B01J31/04 , B01J31/08 , B01J31/22 , C07B61/00 , C07C37/08 , C07C39/07
摘要： PURPOSE:To increase the yield of a cresol from a cymene and facilitate the separation of the cresol from the by-products by converting the primary hydroperoxide and other by-products into the compound which can be recovered as cymene. CONSTITUTION:Cymene is oxidized with oxygen to prepare an oxidation product solution containing the tertiary hydroperoxide and the primary hydroperoxide. The product is treated with hydrogen in the presence of a Pd or Ni catalyst to reduce the primary hydroperoxide, preferably less than 1/25 (w/w), preferably less than 1/50 of the tertiary peroxide. At this time, it is advantageous to maintain the hydrogenation conversion of the tertiary hydroperoxide lower than 30%, preferably lower than 20%. The hydrogen-treated solution is decomposed in the presence of a catalyst, then hydrogenated in the presence of, preferably Pd or copper-chromium catalyst to increase the yield of the cresol.

2. 发明专利

JPH02172941A PRODUCTION OF P-HYDROXYBENZALDEHYDE 失效
公开(公告)号：JPH02172941A
公开(公告)日：1990-07-04
申请号：JP32714788
申请日：1988-12-23
申请人： SUMITOMO CHEMICAL CO
发明人： TAKESHITA AKIRA , TOKUMARU TORU
IPC分类号： B01J31/26 , C07B61/00 , C07C45/81 , C07C47/565
摘要： PURPOSE:To crystallize and separate the subject compound in the form of sodium salt by oxidizing p-cresols in methanol, adding water to the resultant reaction mixture, as necessary, filtering the mixture, then distilling away the methanol, subsequently neutralizing the obtained mixture and cooling the neutralized mixture. CONSTITUTION:p-Cresols are oxidized with oxygen or an oxygen-containing gas in the presence of a catalyst containing sodium hydroxide and a cobalt compound in methanol and water is then added to the resultant reaction mixture. The obtained mixture, as necessary, is filtered to separate tar components, catalyst, etc. The produced solution is then heated to 50-100 deg.C temperature to distill away the methanol. The resultant solution is subsequently neutralized to pH9-11 and, as necessary, extracted with a solvent (the unreacted m-cresol, etc., are separated when mixed m-/p-cresol is used as a raw material) and the solution temperature is then cooled to -20 to +50 deg.C, preferably 0-20 deg.C to crystallize and separate the objective compound in the form of Na salt. The separated crystals are subsequently dissolved in water, as necessary, filtered and neutralized with a mineral acid to crystallize and separate the objective compound.

3. 发明专利

JPH01106838A METHOD FOR PURIFYING P-HYDROXYBENZALDEHYDE 失效
公开(公告)号：JPH01106838A
公开(公告)日：1989-04-24
申请号：JP26354087
申请日：1987-10-19
申请人： SUMITOMO CHEMICAL CO
发明人： TAKESHITA AKIRA , SUZUKI MIKIO , TOKUMARU TORU
IPC分类号： C07C47/565 , C07C45/00 , C07C45/36 , C07C45/80 , C07C67/00
摘要： PURPOSE:To obtain the titled compound from a specific oxidation reaction mixture of p-cresol in high yield, by specifying a raw material reaction ratio in an oxidation step, successively passing the reaction mixture through steps of dilution with water.filtration step, separation of a solvent, neutralization and extraction, distilling and purifying the resultant product. CONSTITUTION:The titled compound is taken out of a reaction mixture obtained by oxidizing p-cresol with oxygen or an oxygen-containing gas in a solvent in the presence of a cobalt compound and base. In the process, the p-cresol reaction ratio in the oxidation step is adjusted to >=92% and the above- mentioned reaction mixture is successively passed through steps of (i) dilution with water and filtration, (ii) separation of the solvent from the afore-mentioned reaction mixture, (iii) neutralization of an aqueous layer after extracting the above-mentioned solvent to pH 3-6 with an acid and (iv), as necessary, separation of the afore-mentioned neutralized solution and extraction of the separated solution with a solvent. The resultant reaction mixture is then distilled and purified to industrially and readily afford the aimed compound useful as an intermediate for medicines, agricultural chemicals, perfumes, etc., in high yield and purity.

4. 发明专利

JPS62270411A METHOD FOR REMOVING PHOSPHORUS OXYCHLORIDE IN THIONYL CHLORIDE 失效
公开(公告)号：JPS62270411A
公开(公告)日：1987-11-24
申请号：JP11168486
申请日：1986-05-15
申请人： SUMITOMO CHEMICAL CO
发明人： OSU MOTOMASA , SUZUKI MIKIO , TOKUMARU TORU
IPC分类号： C01B17/45
摘要： PURPOSE:To obtain high-purity and high-quality thionyl chloride readily and inexpensively, by reacting a mixed solution of thionyl chloride and phosphorus oxychloride with a proper amount of aluminum chloride, distilling and purifying. CONSTITUTION:A mixed solution of thionyl chloride and phosphorus oxychloride simultaneously produced is preferably subjected to relatively simple preparatory distillation and separation and content of phosphorus oxychloride in the mixed solution is reduced to about 0.001-60wt%. The mixed solution is blended with 0.5-10mol, preferably about 1-5mol based on 1mol phosphorus oxychloride of aluminum chloride. The aluminum chloride is preferentially reacted with the phosphorus oxychloride in the mixed solution to form a complex. Then, the mixed solution is distilled and purified, the phosphorus oxychloride is removed while treating the complex as still pot and high-purity and high-quality thionyl chloride is distilled and recovered.

5. 发明专利

JPS6439A PRODUCTION OF 2,4-DICHLORO-3-METHYL-6-TERTIARY BUTYLPHENOL 失效
公开(公告)号：JPS6439A
公开(公告)日：1989-01-05
申请号：JP15599587
申请日：1987-06-22
申请人： SUMITOMO CHEMICAL CO
发明人： TAKESHITA AKIRA , MASAKI SHINZABURO , TOKUMARU TORU , FUJII TAKEO
IPC分类号： B01J27/053 , B01J23/74 , B01J23/745 , B01J27/128 , C07C27/00 , C07C37/62 , C07C39/30 , C07C67/00
摘要： PURPOSE:To selectively obtain the titled compound in good yield, by reacting 3-methyl-4,6-ditertiary butylphenol with chlorine gas in the presence of an iron based catalyst. CONSTITUTION:3-Methyl-4,6-ditertiary butylphenol is reacted with chlorine gas in the presence of an iron based catalyst (e.g. iron, iron oxide or iron sulfate) at 10-50 deg.C, preferably 15-40 deg.C temperature to afford the aimed compound. The amount of the catalyst used is preferably 0.001-0.2mol., preferably 0.01-0.03mol. based on 1mol. raw material compound. The reaction is preferably carried out in a solvent (e.g. a halogenated hydrocarbon) in an amount of 1-5 times based on the raw material compound. The aimed compound is tertiary butylated to provide 2,4-dichloro-3-methylphenol which is a raw material for agricultural chemicals, photographic chemicals, etc.

6. 发明专利

JPS63243046A PRODUCTION OF TERT-BUTYLPHENOLS 失效
公开(公告)号：JPS63243046A
公开(公告)日：1988-10-07
申请号：JP7561087
申请日：1987-03-27
申请人： SUMITOMO CHEMICAL CO
发明人： TAKESHITA AKIRA , MASAKI SHINZABURO , FUJII TAKEO , TOKUMARU TORU
IPC分类号： B01J27/188 , B01J23/28 , B01J23/30 , C07B61/00 , C07C27/00 , C07C37/14 , C07C37/48 , C07C37/50 , C07C39/06 , C07C67/00
摘要： PURPOSE:To obtain mono-tert butylphenols selectivity and in high yield, by reacting a phenol with isobutene or isobutene-containing gas in the presence of a heteropoly acid at a specific temperature and subjecting the reaction product to rearrangement reaction at a specific temperature. CONSTITUTION:A phenol, especially m- or p-cresol, is reacted with isobutene or isobutene-containing gas in the presence of a heteropoly acid, especially tungstosilicic acid at 30-130 deg.C, preferably 40-80 deg.C to a give mono- and di-tert butylphenols. Then the butylphenols are successively subjected to rearrangement reaction at 100-180 deg.C, preferably 105-140 deg.C to give mono-tert butyl phenols such as 4-methyl-6-tert butyl phenol useful as an antioxidant from inexpensive raw materials in high purity, in high yield, industrially and readily while suppressing formation of secondary alkylphenols as by-products.

7. 发明专利

JPS62281887A PRODUCTION OF 0,0-DI LOWER ALKYL CHLOROTHIOPHOSPHATE 失效
公开(公告)号：JPS62281887A
公开(公告)日：1987-12-07
申请号：JP28857686
申请日：1986-12-02
申请人： SUMITOMO CHEMICAL CO
发明人： OSU MOTOMASA , KAMEMOTO KOICHI , TOKUMARU TORU , YAHATA MANABU , HIOKI TAKESHI , UEDA HIROSHI
IPC分类号： C07F9/20
摘要： PURPOSE:To obtain the titled compound useful as an intermediate for agricultural chemicals of organic phosphorous type from readily obtainable inexpensive materials industrially advantageously, by subjecting thiophosphoryl trichloride and a lower alcohol in the presence of caustic soda and water to multi-stage reaction in a specific composition and under a specific condition. CONSTITUTION:In subjecting thiophosphoryl trichloride and a lower alcohol in the presence of caustic soda to multi-stage reaction of 3-8 stages continuously, the total amount of thiophosphoryl trichloride is fed from a feed pipe B to a reaction tank R1, 45-85wt% total amounts of water, caustic soda and the lower alcohol are fed from a feed pipe A1 and the reaction is carried out at

8. 发明专利

JPH0532590A PRODUCTION OF NITROPHENOLS 失效
公开(公告)号：JPH0532590A
公开(公告)日：1993-02-09
申请号：JP19167791
申请日：1991-07-31
申请人： SUMITOMO CHEMICAL CO
发明人： YAMATO MICHIO , TAKAMINE HIROSHI , MURAKAMI AKIRA , TOKUMARU TORU , NAKAYAMA YOSHINORI , HAZAMA YASUO
IPC分类号： C07C201/08 , C07C205/26
摘要： PURPOSE:To industrially and advantageously obtain the subject compounds by reacting 2,4-dichloro-3-alkylphenols with a nitrating agent in a specific solvent. CONSTITUTION:A 2,4-dichloro-3-alkyl-6-t-butylphenol is subjected to removal of the t-butyl group according to transalkylating reaction to provide 2,4- dichloro-3-alkylphenols, which are then subjected to nitrating reaction with a nitric acid solution at 30-98% concentration in an alkylbenzene-based solvent (e.g. toluene), preferably at 20-70 deg.C. The resultant aqueous layer is separated and the organic layer is washed with water. The solvent is subsequently distilled away to afford the objective 2,4-dichloro-3-alkyl-6-nitrophenols.

9. 发明专利

JPS63303941A PRODUCTION OF 2,4-DICHLORO-3-METHYLPHENOL 失效
公开(公告)号：JPS63303941A
公开(公告)日：1988-12-12
申请号：JP14115287
申请日：1987-06-04
申请人： SUMITOMO CHEMICAL CO
发明人： TAKESHITA AKIRA , MASAKI SHINZABURO , FUJII TAKEO , TOKUMARU TORU
IPC分类号： C07C37/50 , C07C27/00 , C07C37/62 , C07C39/30 , C07C67/00
摘要： PURPOSE:To obtain the titled compound, by using 2-chloro-3-methyl-4,6-di-t- butylphenol derived from 3-methyl-4,6-di-t-butylphenol as a raw material and subjecting the raw material to debutylation, chlorination and then removal of t-butyl group. CONSTITUTION:3-Methyl-4,6-di-t-butylphenol is monochlorinated to obtain 2- chloro-3-methyl-4,6-di-t-butylphenol, which is treated with a chlorination agent under heating to effect simultaneous debutylation and chlorination and obtain 2,4-dichloro-3-methyl-6-t-butylphenol. The product is converted to the objective 2,4-dichloro-3-methylphenol by removing t-butyl group. The monochlorination reaction and the treatment with chlorination agent are carried out preferably at 0-50 deg.C and 70-145 deg.C, respectively. The produced compound is useful as a raw material for agricultural chemicals, etc.

10. 发明专利

JPS63264435A PRODUCTION OF P-HYDROXYBENZALDEHYDE 失效
公开(公告)号：JPS63264435A
公开(公告)日：1988-11-01
申请号：JP25553687
申请日：1987-10-08
申请人： SUMITOMO CHEMICAL CO
发明人： OSU MOTOMASA , SUZUKI MIKIO , TOKUMARU TORU , YAHATA MANABU , NISHIZAWA KANJI , HORIKAWA YASUHIKO
IPC分类号： C07C47/36 , C07B61/00 , C07C45/00 , C07C45/36 , C07C47/565 , C07C67/00
摘要： PURPOSE:To obtain, with industrial advantage, the title compound by specifying the oxidation, reactor, the oxygen concentration in the gas phase, the oxygen partial pressure, the agitation power and the depth of the reaction mixture, when p-cresol is oxidized in a solvent in the presence of a cobalt compound and a base. CONSTITUTION:When the title compound is prepared by oxidation of p-cresol or a mixture thereof with oxygen or a gas containing the same in a solvent in the presence of a cobalt compound and a base, an aeration agitation type reactor in which the gas in the reactor space is sucked by rotation of the agitation blades through the agitation hollow shaft into the bottom of the reactor or a reactor in which the reaction mixture at the bottom is recycled with a pump is used for the oxidation and oxygen or a gas containing the same is introduced so that the oxygen concentration in the gas phase becomes 0.1-12% to effect the oxidation at an average oxygen partial pressure of 0.1-2atms, agitation power of 1.5Kw/m , the mixture depth of 0.2-10m. Thus, the subject compound is obtained easily through industrial operation at a high reaction rate in high yield.

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