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1. 发明专利

JPH07285925A METHOD FOR PRODUCING METHYLENE-CROSS-LINKED TRIPHENYLENE TRIISOCYANATE 失效
公开(公告)号：JPH07285925A
公开(公告)日：1995-10-31
申请号：JP7563494
申请日：1994-04-14
申请人： MITSUI TOATSU CHEMICALS
发明人： HONMA SHIRO , TAKASAKI MICHIYA , SHIMAMATSU MITSUNORI , IIJIMA MASAAKI , SATO NAOKI , MIYATA KATSUJI
IPC分类号： C07C263/20 , C07C265/14
摘要： PURPOSE:To isolate a trinuclear compound in a high yield and in a high purity, while reducing the by-production of tar, by subjecting a methylene-cross-linked polyphenylene polyisocyanate mixture to the combination of specific separation methods comprising specified operation conditions. CONSTITUTION:A methylene-cross-linked triphenylene triisocyanate of the formula wherein n is 1 is isolated from the mixture of methylene-cross-linked polyphenylene polyisocyanates of the formula wherein n is 0 or a positive integer. Namely, most of diphenylmethane diisocyanate compound contained in the mixture is distilled off or evaporated off with a thin film evaporator. Subsequently, the methylene-cross-linked triphenylene triisocyanate is isolated and purified with a thin film evaporator. Or a methylene-cross-linked polyphenylene polyisocyanate fraction containing the diphenylmethane diisocyanate and the methylene-cross-linked triphenylene isocyanate as main components is obtained from the mixture with the above-mentioned device, and the diphenylmethane diisocyanate is distilled off from the low boiling point fraction.

2. 发明专利

JPH08151422A PRODUCTION OF METHYLENE-BRIDGED POLYPHENYLENEPOLYAMINE 失效
公开(公告)号：JPH08151422A
公开(公告)日：1996-06-11
申请号：JP29277294
申请日：1994-11-28
申请人： MITSUI TOATSU CHEMICALS
发明人： IIJIMA MASAAKI , SATO NAOKI , TANIGUCHI TOSHIYUKI , SHIMAMATSU MITSUNORI , KURODA KAZUMOTO , MIYATA KATSUJI
IPC分类号： C08G12/08 , C07C209/78 , C07C211/49 , C08G18/76
摘要： PURPOSE: To produce a high-performance polyamine of a specified composition in a manner that the control of the composition of components with the different numbers of nuclei is possible by condensing aniline with formaldehyde in the presence of an acid catalyst and 2,4'-diaminodiphenylmethane. CONSTITUTION: This process is one for producing methylene-bridged polyphenylenepolyamine by condensing aniline with formaldehyde in the presence of an acid catalyst, wherein 2,4'-diaminodiphenylmethane is added to the system. This condensation is conducted at 10-40 deg.C. It is suitable that the molar ratio of the formaldehyde to the aniline is 1-3 and that the molar ratio of the aniline to the acid catalyst is 0.1-1. It is particularly desirable that the aniline/ formaldehyde molar ratio is 2.2-2.6 and that the acid/aniline molar ratio of 0.3-0.5. According to this process, the control of components of the different numbers of nuclei is possible (for example the amount of trinuclear component formed becomes larger, and the ratio of trinuclear component/at least tetranulear component ratio and the tetranuclear component/at least pentanuclear component ratio can be heightened by simply changing the amount of o-p' MDA added.

3. 发明专利

JPH0665164A PRODUCTION OF CYCLOHEXANE-1,2-DIAMINES 失效
公开(公告)号：JPH0665164A
公开(公告)日：1994-03-08
申请号：JP22288192
申请日：1992-08-21
申请人： MITSUI TOATSU CHEMICALS
发明人： AKIEDA HIDEYUKI , SHIMAMATSU MITSUNORI , KURODA KAZUMOTO , NITTA KAZUNARI
IPC分类号： B01J23/42 , C07B61/00 , C07C209/62 , C07C211/36
摘要： PURPOSE:To obtain the subject compound useful as an epoxy curing agent, a chelating agent, etc., efficiently and in high yield by hydrogenating a specific benzimidazolinone compound in an organic solvent in the presence of a catalyst of platinum oxide under a specific condition and hydrolyzing. CONSTITUTION:A benzimidazolinone compound of the formula (R is 1-5C alkyl) such as 4-methyl-benzimidazolinone is subjected to nucleus hydrogenation in an organic solvent such as acetic acid in the presence of a catalyst of platinum oxide under 5-100kg/cm G hydrogen pressure at 25-80 deg.C and a prepared cyclohexaneimidazolinone compound is further hydrolyzed to give the objective compound.

4. 发明专利

JPH07316123A PRODUCTION OF METHYLENE-CROSSLINKED POLYPHENYLENE POLYISOCYANATE 失效
公开(公告)号：JPH07316123A
公开(公告)日：1995-12-05
申请号：JP10817194
申请日：1994-05-23
申请人： MITSUI TOATSU CHEMICALS
发明人： TAKASAKI MICHIYA , SHIMAMATSU MITSUNORI , TANIGUCHI TOSHIYUKI , HONMA SHIRO , SATO NAOKI , KURODA KAZUMOTO , OTSUBO KENJI
IPC分类号： C07C263/10 , C07C263/20 , C07C265/14 , C08G18/76
摘要： PURPOSE:To provide a process for producing the compound having freely controllable nucleus composition and utilizable for the production of polyurethane foam, elastomer, adhesive, coating, etc. CONSTITUTION:A mixture of isocyanates of formula ((n) is 0 or positive integer) is used as a raw material, charged into an extractor together with 0.2-50 pts.wt., preferably l-10 pts.wt. (based on 1 pt.wt. of the raw material) of a solvent consisting of an aliphatic hydrocarbon, an alicyclic hydrocarbon or their mixture and extracted at 10-80 deg.C, preferably 25-50 deg.C. The system is separated into the extracted phase and the residual phase and the solvent is distilled off from the extracted phase to obtain a methylene-crosslinked polyphenylene polyisocyanate containing =5-nucleus compound and having a trinucleus compound/>=4-nucleus compounds of >=1.2. The nucleus composition is controlled mainly by controlling the extraction temperature.

5. 发明专利

JPH02261816A PREPARATION OF URETHANE PREPOLYMER FOR COATING 失效
公开(公告)号：JPH02261816A
公开(公告)日：1990-10-24
申请号：JP8158089
申请日：1989-04-03
申请人： MITSUI TOATSU CHEMICALS
发明人： NAGO TAKU , OKAWA YUICHI , TANIGUCHI TOSHIYUKI , SHIMAMATSU MITSUNORI , TAKENAKA SHINJI , KURODA KAZUMOTO
IPC分类号： C09D175/04 , C08G18/10 , C08G18/32 , C09D175/00
摘要： PURPOSE:To prepare the subject prepolymer with excellent storage stability in various solvent for a long time by incorporating trimethylolpropane in a reaction soln. contg. a specific prepolymer contg. terminal hydroxyl groups and reacting it with excess tolylene diisocyanate. CONSTITUTION:In a method for reacting a diol and trimethylolpropane with tolylene diisocyanate, after 2mol or more of the diol (e.g. ethylene glycol or 1,3-butanediol) is reacted with tolylene diisocyanate to prepare a prepolymer having hydroxyl groups on its terminals, trimethylolpropane is mixed with the reaction mixture, or separately excess tolylene diisocyanate is reacted with hydroxyl groups to prepare a urethane prepolymer, and unreacted tolylene diisocyanate is removed. The reaction product is dissolved in an ester such as ethyl acetate or an arom. hydrocarbon solvent such as toluene to obtain the subject improve prepolymer which can be stored stably for a long time.

6. 发明专利

JPH07316122A PRODUCTION OF METHYLENE-CROSSLIKED POLYPHENYLENE POLYISOCYANATE 失效
公开(公告)号：JPH07316122A
公开(公告)日：1995-12-05
申请号：JP11245194
申请日：1994-05-26
申请人： MITSUI TOATSU CHEMICALS
发明人： ISHIDA NORITOSHI , SHIMAMATSU MITSUNORI , KURODA KAZUMOTO , MIYATA KATSUJI
IPC分类号： C07C263/10 , C07B61/00 , C07C265/14 , C08G18/76
摘要： PURPOSE:To provide a process for the production of a methylene-crosslinked polyphenylene polyisocyanate having low acid and hydrolyzable chlorine contents and excellent hue. CONSTITUTION:A methylene-crosslinked polyphenylene polyisocyanate is produced by condensing aniline with formaldehyde and reacting the produced polyamine mixture with phosgene in an inert solvent in the presence of an acid catalyst. In the above process, the phosgenation is carried out at

7. 发明专利

JPH04159259A PRODUCTION OF METHYLENE-CROSSLINKED POLYPHENYLENE POLYISOCYANATE 失效
公开(公告)号：JPH04159259A
公开(公告)日：1992-06-02
申请号：JP28351590
申请日：1990-10-23
申请人： MITSUI TOATSU CHEMICALS
发明人： ISHIDA NORITOSHI , TAJIMA JUNJI , SHIMAMATSU MITSUNORI , NITTA KAZUNARI , NAGO TAKU
IPC分类号： C07C263/10 , C07C263/20 , C07C265/14 , C08G18/76
摘要： PURPOSE:To obtain highly reactive poly-MDI and high-purity 4,4'-MDI simultaneously by separating the product obtained by reaction of a polyamine with phosgene into a MDI isomer mixture and poly-MDI through distillation and by further separating the isomer mixture through crystallization. CONSTITUTION:A product obtained by reaction with phosgene of a polyamine formed by condensation between aniline and formalin in the presence of an acid catalyst, is distilled and separated into (A) a mixture of various isomers of diphenylmethane diisocyanate (MDI) and (B) a methylene-crosslinked polyphenylene polyisocyanate (poly-MDI) containing 20-60wt.% of MDI. The mixture A is then separated, through a crystallization process, into (C) 10-40wt.% of a uncrystallized portion with acid and hydrolyzable chlorine highly concentrated, (D) 10-40wt.% of an initial soluble portion and (E) 40-60wt.% of the main soluble portion comprising high-purity 4,4'-MDI, and an inert gas is introduced into the component C followed by treatment under heating at 80-120 deg.C and then mixing with the component B at an arbitrary proportion.

8. 发明专利

JPH04154744A PRODUCTION OF METHYLENE-CROSSLINKED POLYARYLAMINE 失效
公开(公告)号：JPH04154744A
公开(公告)日：1992-05-27
申请号：JP27790790
申请日：1990-10-18
申请人： MITSUI TOATSU CHEMICALS
发明人： TAJIMA JUNJI , SHIMAMATSU MITSUNORI , ISHIDA NORITOSHI , NITTA KAZUNARI , NAGO TAKU
IPC分类号： C07C209/78 , C07C209/86 , C07C211/50
摘要： PURPOSE:To obtain the subject compound from aniline and formaldehyde at a low cost by extracting and separating an aqueous layer separated from a reaction product with a water-insoluble organic solvent, separating and recovering the solvent, aniline and the subject compound from the solvent layer and recycling the materials to the reaction system. CONSTITUTION:The subject compound is produced by (1) condensing aniline and formaldehyde using hydrochloric acid as a catalyst and neutralizing the condensation product with excess sodium hydroxide based on the used hydrochloric acid, (2) separating the obtained reaction product into an aqueous layer and an oil layer by allowing to stand the reaction product and washing the oil layer with water and (3) separating the product into layers and finally removing water and aniline from the layer by an aniline-removing process. In the above process, the oil component in the aqueous layers (i) and (ii) separated from the reaction product is extracted with an essentially water-insoluble organic solvent, the extraction product is separated (4), the solvent (c), aniline and the objective compound are separated and recovered (3) from the solvent layer (v) and each component is recycled to extraction step (4), condensation step (1) or aniline-removal step. The organic material content in waste water can be decreased and the recovery of aniline and the yield of the objective compound can be improved.

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