公开(公告)号：JPH072990A

公开(公告)日：1995-01-06

申请号：JP14736593

申请日：1993-06-18

Applicant: MITSUI TOATSU CHEMICALS

Inventor： YASUI OSAMU ,  OBUCHI SEIJI ,  OTA MASAHIRO

IPC: C08G63/06 ,  C08G63/78 ,  C08L101/16

Abstract: PURPOSE:To industrially and inexpensively obtain a high-mol. weight poly(hydroxy carboxylic acid) in a short time through direct polycondensation with dehydration. CONSTITUTION:The production process comprises heating a hydroxy carboxylic acid or an oligomer thereof in an organic solvent under reflux in the presence of a catalyst to remove the formed water and low-boiling compounds from the reaction system, and then conducting polycondensation with dehydration while refluxing the solvent and simultaneously removing the formed water from the system, the solvent being an aliphatic hydrocarbon.

公开(公告)号：JPH06200042A

公开(公告)日：1994-07-19

申请号：JP34821092

申请日：1992-12-28

Applicant: MITSUI TOATSU CHEMICALS

Inventor： MORI YUKIKO ,  FUKUIRI YASUSHI ,  OBUCHI SEIJI ,  OTA MASAHIRO

IPC: C08J3/14

Abstract: PURPOSE:To produce particles having a uniform particle diameter and freed from fine powder without using any special apparatus by forming the title particles in the first tank, distilling off the organic solvent from the mixture, sending the particles to the second and subsequent tanks, and distilling off the residual organic solvent and poor solvent. CONSTITUTION:At least two granulation tanks are used. In the first tank, a suspended mixture comprising water, an organic solvent solution of a polycarbonate and a poor solvent for the polycarbonate is heated under agitation to form polycarbonate particles; an organic solvent solution of the polycarbonate and an aqueous solution of the poor solvent are continuously fed to the mixture; and the organic solvent for the polycarbonate is distilled off to form polycarbonate particles. The obtained particles are sent to the second and subsequent tanks to distill off the residual solvent and poor solvent, and the obtained particles are continuously withdrawn to produce polycarbonate particles. Thus, a high-bulk-density fine-powder-free particles with a uniform particle diameter can be obtained without using any special apparatus.

公开(公告)号：JPH06192413A

公开(公告)日：1994-07-12

申请号：JP34632892

申请日：1992-12-25

Applicant: MITSUI TOATSU CHEMICALS

Inventor： GOTO KENICHI ,  KIYOMIYA TATSUYA ,  OBUCHI SEIJI ,  OTA MASAHIRO

IPC: C08G64/24 ,  C08G64/20 ,  C08G64/22

Abstract: PURPOSE:To efficiently produce several kinds of arom. polycarbonates having different mol.wts., processibilities, and mechanical characteristics simultaneously on a single production line. CONSTITUTION:A soln. obtd. by dissolving at least one arom. dihydroxy compd. in an aq. soln. of an alkali or alkaline earth metal salt is reacted with a carbonyl halide compd. in the presence of a polymn. catalyst, a mol.-wt.- adjusting agent, and an org. solvent. These raw materials are continuously fed into a reactor comprising at least three reaction vessels installed in series, where the reaction is carried out under such conditions that the dwell time in each vessel is kept constant and that the component dwelling in the reactor is continuously taken out of at least two arbitrarily selected vessels including the last vessel.

公开(公告)号：JPH06145638A

公开(公告)日：1994-05-27

申请号：JP29504692

申请日：1992-11-04

Applicant: MITSUI TOATSU CHEMICALS

Inventor： MATSUYAMA AKIO ,  KOUGO OSAMU ,  OTA MASAHIRO

IPC: C08G73/10 ,  C09J179/08

Abstract: PURPOSE:To obtain a heat-resistant adhesive comprising a specific polyamic acid and a specific bismaleimide compound in a specified ratio, excellent in tensile shear adhesive strength and T shape release adhesive strength, and useful for polyimide films, etc. CONSTITUTION:This adhesive comprises (A) 100 pts.wt. of a polyamic acid obtained by polymerizing (i) 10-50mol.% of an aromatic diamine compound of formula I (X1 is direct bond, 1-10C divalent hydrocarbon, hexafluorinated isopropylidene, etc.,) and (ii) 50-90mol.% of an aromatic diamine of formula II (X2 is direct bond, 1-10C divalent hydrocarbon, etc.,) with (iii) a tetracarboxylic acid dianhydride of formula III (Y is tetravalent group) and (B) 0.1-5 pts.wt. of a bismaleimide compound of formula IV [R is m-phenylene, group of formula V (Z is direct, 1-10C divalent hydrocarbon, etc.,].

公开(公告)号：JPH06116381A

公开(公告)日：1994-04-26

申请号：JP27147792

申请日：1992-10-09

Applicant: MITSUI TOATSU CHEMICALS

Inventor： OBUCHI SEIJI ,  OTA MASAHIRO

IPC: C08G63/06 ,  C08G63/88 ,  C08G63/90

Abstract: PURPOSE:To efficiently remove a catalyst contained in the subject polymer useful as a medical material, etc., by a simple method by bringing a solid substance of a polyhydroxycarboxylic acid into contact with an acidic substance in the presence of a hydrophilic organic solvent. CONSTITUTION:A solid substance of a polyhydroxycarboxylic acid of the formula (R1 to R4 are H or 1-6C saturated hydrocarbon; (a) and (b) are 0 or 1-6 with the proviso that (a) and (b) are not 0 at the same time; (m) and (n) are 0 or 1 or more with the proviso that (m) and (n) are not 0 at the same time) having 0.1-5dl/g intrinsic viscosity is brought into contact with an acidic substance (preferably hydrochloric acid or sulfuric acid) in the presence of a hydrophilic organic solvent (preferably alcohol) preferably at 0-60 deg.C for 0.5-8 hours. The polyhydroxycarboxylic acid, for example, is obtained by direct polymerization through dehydration of an aliphatic hydroxycarboxylic acid such as glycolic acid.

公开(公告)号：JPH06100535A

公开(公告)日：1994-04-12

申请号：JP25282592

申请日：1992-09-22

Applicant: MITSUI TOATSU CHEMICALS

Inventor： YOSHIDA IKUNORI ,  OBUCHI SEIJI ,  OTA MASAHIRO

IPC: B01J23/04 ,  B01J27/02 ,  B01J31/02 ,  C07B61/00 ,  C07D207/452

Abstract: PURPOSE:To obtain a bismaleimide in high efficiency in a short time by reacting a diamine compound with maleic anhydride by azeotropic dehydration process using a specific mixed solvent as the reaction solvent. CONSTITUTION:A bismaleimide of formula II is produced by reacting a diamine compound of formula I (X is direct bond, 1-20C bivalent hydrocarbon group, hexafluorinated isopropylidene, carbonyl, thio or sulfonyl; the position of N atom is p-, o- or m- relative to X; Y1 to Y4 are H, lower alkyl, lower alkoxy, Cl or Br) with maleic anhydride in the presence of an acidic or basic catalyst in a reaction solvent consisting of a mixed solvent obtained by mixing 100 pts. of an organic solvent capable of forming an azeotropic mixture with water (e.g. hexane or toluene) with >=15 pts. of an aprotic polar organic solvent (e.g. N,N-dimethylformamide) while removing the produced water from the system under heating and refluxing. The amount of the catalyst can be reduced, the recovery of the solvent can be simplified and the volumetric efficiency of the reactor can be improved compared with a conventional synthetic process.

公开(公告)号：JPH0649360A

公开(公告)日：1994-02-22

申请号：JP20112892

申请日：1992-07-28

Applicant: MITSUI TOATSU CHEMICALS

Inventor： MATSUYAMA AKIO ,  OTA MASAHIRO

IPC: C08L79/08 ,  C09D179/08 ,  C09J179/08

Abstract: PURPOSE:To obtain an aqueous polyamic acid solution being moldable at low temperatures, having excellent adhesive strength and not polluting the working environment by mixing a specified amount of a specified polyamic acid with a basic compound. CONSTITUTION:2-40wt.% polyamic acid of the formula (wherein X is -CO- or -SO2-; and R is a tetravalent group selected from among a 2 C or higher aliphatic group, a cycloaliphatic group, a monocyclic aromatic group, a fused polycyclic aromatic group and a nonfused polycyclic aromatic group consisting of aromatic groups bonded to each other directly or through bridging members) is mixed with a basic compound (e.g. ammonia) desirably in an amounts satisfying the relationship: 0.5Ma

公开(公告)号：JPH0625151A

公开(公告)日：1994-02-01

申请号：JP18490992

申请日：1992-07-13

Applicant: MITSUI TOATSU CHEMICALS

Inventor： OBUCHI SEIJI ,  FUKUIRI YASUSHI ,  OTA MASAHIRO

IPC: B01J23/745 ,  B01J23/74 ,  B01J27/049 ,  B01J27/128 ,  B01J27/185 ,  B01J27/25 ,  C07B61/00 ,  C07C319/08 ,  C07C321/26 ,  C07C323/09

Abstract: PURPOSE:To obtain in high yield and purity at low cost the subject compound useful as an intermediate for near-infrared absorbers requiring no purification by extracting a dithiol complex under specified conditions. CONSTITUTION:A halogen-substituted benzene compound of formula I (X is Cl or Br; R1-R4 are each H, Cl, 1-3C alkyl, alkenyl, alkoxy, aryl, etc.) is made to react with a hydrosulfide in the presence of iron sulfide and an iron salt in a solvent (e.g. N,N-dimethylformamide) at 60-140 deg.C to form a complex of iron or its salt and a dithiol compound. This complex is then treated under heating with a metal oxide, alkali metal hydroxide or alkaline earth metal hydroxide. Next, the product is filtered, and an mineral acid is added to the resulting filtrate to deposit crystal, which is then extracted with an organic solvent (e.g. dichloromethane), thus obtaining the objective compound of formula II, e.g. 3,4,6-trichlorobenzene-1,2-dithiol.

公开(公告)号：JPH05202187A

公开(公告)日：1993-08-10

申请号：JP1078592

申请日：1992-01-24

Applicant: MITSUI TOATSU CHEMICALS

Inventor： OTA MASAHIRO ,  MATSUYAMA AKIO ,  KUWANO FUMIAKI ,  SEGAMI EIJI ,  YASUI OSAMU ,  YOSHIDA IKUNORI ,  RYU AKINORI

IPC: C08G73/10

Abstract: PURPOSE:To obtain the subject precursor by reacting a tetracarboxylic acid dianhydride with a diamine compound in a specific temperature range, having sufficient molecular weight, proper mechanical viscosity and good workability. CONSTITUTION:(A) A tetracarboxylic acid dianhydride of formula I (R is >=2C aliphatic, cycloaliphatic, monocyclic aromatic or condensed polycyclic aromatic group) such as ethylenetetracarboxylic acid dianhydride is reacted with (B) a diamine compound of formula II (R' is >=2C aliphatic, monocyclic aromatic or cycloaliphatic group) such as 1,2-phenylenediamine in an organic solvent at 40-100 deg.C to give the objective precursor suitable for film, wire coating varnish, cover lay, adhesive, etc.

公开(公告)号：JPH05178828A

公开(公告)日：1993-07-20

申请号：JP756992

申请日：1992-01-20

Applicant: MITSUI TOATSU CHEMICALS

Inventor： OTA MASAHIRO ,  MATSUYAMA AKIO ,  KUWANO FUMIAKI ,  SEGAMI EIJI ,  YASUI OSAMU ,  YOSHIDA IKUNORI ,  RYU AKINORI ,  KOBAYASHI TADASHI

IPC: C07D209/48 ,  C07D209/66 ,  C08K5/3412 ,  C08K5/3417 ,  C08L79/08

Abstract: PURPOSE:To provide an aromatic bisimide compound giving a polyimide molding resin composition having fluidity in molten state and excellent processability in addition to the characteristic heat-resistance of polyimide. CONSTITUTION:The bisimide compound of formula I [A is group of formula II (X is direct bond, bivalent hydrocarbon group, hexafluorinated isopropylidene, carbonyl, thio or sulfonyl; 1 to Y4 are H, alkyl, alkoxy, Cl or Br), CO or group of formula III to formula V; R is monocyclic aromatic group, condensed polycyclic aromatic group or non-condensed polycyclic aromatic group]. A molding polyimide resin composition can be prepared by compounding 0.5-100 pts.wt. of the compound of formula I to 100 pts.wt. of a polyimide having the recurring structural unit of formula VI (R' is >=2C aliphatic group, cycloaliphatic group, monocyclic aromatic group or condensed or non-condensed polycyclic aromatic group). A carbon fiber-reinforced polyimide resin composition is produced by compounding a polyimide with carbon fibers surface-coated with the compound of formula I. The compound of formula I can be produced by reacting the corresponding diamine compound with a dicarboxylic acid anhydride.