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    SEPARATION AND PURIFICATION OF BIPHENYL-4,4'-DIOL
    22.
    发明专利
    SEPARATION AND PURIFICATION OF BIPHENYL-4,4'-DIOL 失效

    公开(公告)号：JPH0426640A

    公开(公告)日：1992-01-29

    申请号：JP12665390

    申请日：1990-05-18

    Applicant: TOSOH CORP

    Inventor： YOSHIMITSU MITSUAKI ,  KUBO MASAJI

    IPC: B01D11/02 ,  C07C37/72 ,  C07C37/78 ,  C07C39/15

    Abstract: PURPOSE:To obtain the title high-purity compound in a short time, by extracting crude biphenyl-4,4'-diol with an organic solvent, dripping the solution into hot water and recovering the title compound as powder dispersed into water while simultaneously distilling away the solvent. CONSTITUTION:Crude biphenyl-4,4'-diol is extracted with an organic solvent (preferably alcohols or ketones which can be distilled or subjected to azeotropic distillation with water especially at

    PRODUCTION OF HEXABROMOCYCLODODECANE
    23.
    发明专利
    PRODUCTION OF HEXABROMOCYCLODODECANE 失效

    公开(公告)号：JPH03218330A

    公开(公告)日：1991-09-25

    申请号：JP28845290

    申请日：1990-10-29

    Applicant: TOSOH CORP

    Inventor： MATSUBA TAKAO ,  KUBO MASAJI ,  KAWAHATA KOUJI

    IPC: C07C17/02 ,  C07C23/02

    Abstract: PURPOSE:To obtain gamma-form of title substance in high yield by dropwisely adding 1,5,9-cis, trans, trans-cyclododecatriene to a lower alcohol or organic solvent containing the lower alcohol in which bromine is dissolved to react bromine with the above-mentioned cyclododecatriene. CONSTITUTION:1,5,9-cis, trans, trans-Cyclododecatriene(CDT) is dropwisely added to 1-4C alcohol (preferably ethanol, n-propanol or tert.-butanol) or organic solvent containing the same alcohol in which bromine is dissolved and reacted with bromine at-20-50 deg.C to provide gamma-form of title substance useful as flame- retardant for high polymer compound in high selectivity and yield. The objective compound having excellent hue and heat stability is obtained, because the production of impurities is reduced. Molar ratio of bromine/CDT is preferably 3.0-10.0 and CDT concentration to the organic solvent is preferably 0.1-40wt./vol.%.

    PRODUCTION OF TETRABROMOBISPHENOL A
    24.
    发明专利
    PRODUCTION OF TETRABROMOBISPHENOL A 失效

    公开(公告)号：JPH03209340A

    公开(公告)日：1991-09-12

    申请号：JP257690

    申请日：1990-01-11

    Applicant: TOSOH CORP

    Inventor： EGUCHI HISAO ,  KUBO MASAJI ,  KUNIMOTO KOJI

    IPC: C07C37/62 ,  C07C39/367

    Abstract: PURPOSE:To obtain the subject compound having high quality and decreased content of hydrolyzable bromine and inorganic bromide ion, on an industrial scale at a low cost, by brominating bisphenol A with bromine in methanol while specifying the substrate concentration of the above raw material relative to methanol. CONSTITUTION:Tetrabromobisphenol A useful as a flame-retardant for epoxy resin and ABS resin is produced by brominating bisphenol A with bromine in methanol. In the above process, the substrate concentration of bisphenol A relative to methanol is adjusted to 0.1-10w/v%, preferably 1-8w/v% to obtain the objective compound having high quality. Since the product has remarkably decreased contents of hydrolyzable bromine and inorganic bromine ion, it can be used, without necessitating particular purification process, as a flame- retardant for resin for electrical and electronic use such as laminated sheet or sealant. The compound can be produced on an industrial scale at a low cost with a simplified process compared with conventional process.

    PRODUCTION OF BIS(4-HYDROXY-3,5-DIBROMOPHENYL)SULFONE
    26.
    发明专利
    PRODUCTION OF BIS(4-HYDROXY-3,5-DIBROMOPHENYL)SULFONE 失效

    公开(公告)号：JPH03153662A

    公开(公告)日：1991-07-01

    申请号：JP29249789

    申请日：1989-11-13

    Applicant: TOSOH CORP

    Inventor： SAKKA HIDEO ,  SHIMIZU SADAMI ,  EGUCHI HISAO ,  KUBO MASAJI

    IPC: B01J23/04 ,  B01J27/232 ,  C07B61/00 ,  C07C315/04 ,  C07C317/22

    Abstract: PURPOSE:To produce the high-purity title compound in high yield without using an oxidizing agent by adding a certain amount of bromine and inorganic metal base to bis(4-hydroxyphenyl)solfone to carry out reaction when bis(4- hydroxyphenyl)sulfone is brominated in a mixed solvent of water and alcohol. CONSTITUTION:When bis(4-hydroxyphenyl)sulfone (hereinafter referred to as BPS) expressed by formula I is brominated with bromine, the reaction is carried out by adding bromine of 4.0-5.0mol and inorganic metal salt of 2.0-4.0 gram equivalent based on 1mol BPS to BPS to provide the bis(4-hydroxy-3,5- dibromophenyl)sulfone (hereinafter referred to as TBS) expressed by formula II. The reaction is industrially advantageous without requiring addition of an oxidizing agent and high purity and high yield is attainable in a short time. TBS is utilized as a flameretardant and raw material for flame-retardant of polyolefin-resin, etc., without special purification process.

    PREPARATION OF BIPHENYL-4,4'-DIOL
    29.
    发明专利
    PREPARATION OF BIPHENYL-4,4'-DIOL 失效

    公开(公告)号：JPH0338538A

    公开(公告)日：1991-02-19

    申请号：JP17187689

    申请日：1989-07-05

    Applicant: TOSOH CORP

    Inventor： OGAWA TSUKASA ,  KUBO MASAJI ,  YOSHIMITSU MITSUAKI

    IPC: C07C37/02 ,  C07B61/00 ,  C07C39/15

    Abstract: PURPOSE:To prepare the subject compound at low temperature in a short time and in high selectivity by performing the hydrolysis of a 4,4'-dihalogenobiphenyl in an alcohol-containing aqueous solution in the presence of an aliphatic compound such as diethylene glycol, the halogen being chlorine and/or bromine. CONSTITUTION:When a 4,4'-dihalogenobiphenyl is hydrolyzed with an alkali metal hydroxide in the presence of a monovalent and/or divalent copper compound catalyst to prepare biphenyl-4,4'-diol, the halogen being bromine and/or bromine, the hydrolysis reaction is performed in the presence of an aliphatic compound of the formula ((n) is 1-40; R is H or 1-40C alkyl) (e.g. diethylene glycol or ethylene glycol) in a 1-3C monovalent alcohol-containing aqueous solution. The method does not require the large load of a purification process and permits to avoid the corrosion of a metal installation material.

    SYNTHESIS OF BIPHENYL-4,4'-DIOL
    30.
    发明专利
    SYNTHESIS OF BIPHENYL-4,4'-DIOL 失效

    公开(公告)号：JPH0338537A

    公开(公告)日：1991-02-19

    申请号：JP17187589

    申请日：1989-07-05

    Applicant: TOSOH CORP

    Inventor： OGAWA TSUKASA ,  KUBO MASAJI ,  YOSHIMITSU MITSUAKI

    IPC: C07C37/02 ,  C07B61/00 ,  C07C39/15

    Abstract: PURPOSE:To prepare the subject compound at low temperature in a short time and in high selectivity by performing the hydrolysis of a 4,4'-dihalogenobiphenyl in the presence of trietylenediamine in an alcohol-containing aqueous solution, the halogen being chlorine and/or bromine. CONSTITUTION:When a 4,4'-dihalogenobiphenyl is hydrolyzed with an alkali metal hydroxide in the presence of a monovalent and/or divalent copper compound catalyst to prepare biphenyl-4,4'-diol, the halogen being chlorine and/or bromine, the hydrolysis reaction is performed in the presence of triethylenediamine in an alcohol-containing aqueous solution. The method permits to finish the hydrolysis reaction in a short time at a low temperature of

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