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    Novel spiro compound
    3.
    发明专利
    Novel spiro compound 失效
    新型SPIRO化合物

    公开(公告)号：JPS59216889A

    公开(公告)日：1984-12-06

    申请号：JP8997483

    申请日：1983-05-24

    Applicant: Daicel Chem Ind Ltd

    Inventor： HATSUTORI SHINJI

    IPC: C07D493/10 ,  C08G59/00 ,  C08G59/02 ,  C08G59/20

    Abstract: NEW MATERIAL:3-Cyclohexenyl-9-( 3,4-oxycyclohexanyl )2,4,8,10-tetraoxaspiro[5, 5]undecane of formula I and/or 3,9-di(3,4-oxycyclohexanyl)2,4,8,10-tetraoxaspiro [5,5]undecane.
    USE: A starting material of spiran resins: especially, it is suitable for a starting material of a powder resin used in transfer molding.
    PREPARATION: 1,2,5,6-Tetrahydrobenzaldehyde resultant from Diels-Alder reaction between butadiene and acrolein is acetalized with pentaerythritol to form 3,9-dicyclohexenyl-2,4,8,10-tetraoxaspiro[5,5]undecane. Then, the product is epoxidized with a peracid such as performic acid.
    COPYRIGHT: (C)1984,JPO&Japio

    Abstract translation: 新材料：式I的3-环己烯基-9-（3,4-氧基环己基）2,4,8,10-四氧杂螺[5,5]十一烷和/或3,9-二（3,4-氧基环己基）2 ，4,8,10-四氧杂螺[5,5]十一烷。 用途：螺旋树脂的起始原料：特别适用于传递成型中使用的粉末树脂的原料。 制备：由丁二烯和丙烯醛之间的Diels-Alder反应产生的1,2,5,6-四氢苯甲醛用季戊四醇缩醛化形成3,9-二环己烯基-2,4,8,10-四氧杂螺[5,5]十一烷。 然后，产物用过酸（如过酸）环氧化。

    Purification of epoxy compound
    6.
    发明专利
    Purification of epoxy compound 失效
    环氧化合物的纯化

    公开(公告)号：JPS59101476A

    公开(公告)日：1984-06-12

    申请号：JP21022782

    申请日：1982-11-30

    Applicant: Daicel Chem Ind Ltd

    Inventor： HATSUTORI SHINJI

    IPC: C07D301/32

    Abstract: PURPOSE: To purify a crude epoxy compound having small boiling temperature difference between acetic acid, thermally unstable in the presence of acetic acid, and unsuitable for the application of water extraction process, in high yield, by combining a flash evaporation process with a fractional condensation process.
    CONSTITUTION: A crude epoxy compound is charged in a flash evaporator having short residence time, e.g. a thin-film evaporator, and subjected to the flash evaporation under reduced pressure. The temperature of the heat medium in the flash evaporator is adjusted preferably at a level lower than the boiling point of the epoxy compound under the corresponding vapor pressure by 10W40°C. The vapor generated by the flash evaporation is partially condensed in the first condenser, and the condensed liquid containing concentrated epoxy compound is recycled as a feed liquid. The noncondensed vapor is introduced into the second condenser, condensed completely, the recovered as an acetic acid solution. The epoxy compound suitable for the process is the one having a boiling temperature difference of 50W150°C betweeen acetic acid.
    COPYRIGHT: (C)1984,JPO&Japio

    Abstract translation: 目的：为了纯化乙酸之间沸点差小的粗环氧化合物，在乙酸存在下热不稳定，并且不适于施用水提取过程，以高产率，通过将闪蒸法与分级缩合 处理。 构成：将粗环氧化合物装入具有短停留时间的闪蒸器中，例如， 薄膜蒸发器，并在减压下进行闪蒸。 闪蒸器中的热介质的温度优选在相对蒸气压10-40℃下比环氧化合物的沸点低。 由闪蒸产生的蒸汽在第一冷凝器中部分冷凝，含有浓缩环氧化合物的冷凝液作为进料液循环。 将非冷凝蒸汽引入第二冷凝器中，完全冷凝，以乙酸溶液回收。 适用于该方法的环氧化合物是在乙酸之间的沸点差为50-150℃的环氧化合物。

    Preparation of novolak epoxy resin
    9.
    发明专利
    Preparation of novolak epoxy resin 失效
    NOVOLAK环氧树脂的制备

    公开(公告)号：JPS5966414A

    公开(公告)日：1984-04-14

    申请号：JP17719382

    申请日：1982-10-08

    Applicant: Daicel Chem Ind Ltd

    Inventor： WATANABE MASAHARU ,  HATSUTORI SHINJI ,  YANAGII TOYOKAZU

    IPC: C08G8/00 ,  C08G8/28 ,  C08G59/00 ,  C08G59/20 ,  C08G59/34

    Abstract: PURPOSE: To obtain a novolak epoxy resn useful for sealing up electrical insulating materials and semiconductors with almost no residual halogens, by epoxidizing an allyl etherified novolak resin in a liquid phase with an organic peracid.
    CONSTITUTION: An allyl etherified novolak resin, e.g. a resin obtained by synthesizing a novolak resin from phenol or cresol and formalin, and reacting the resultant novolak resin with an allyl halide in the presence of an alkali hydroxide is dissolved in a solvent, e.g. hexane, and reacted with a solution of an organic peracid, preferably peracetic acid, preferably at 40W70°C reaction temperature. The resultant reacion solution is subjected to the removal of the solvent and the organic acid and if necessary desalting (to remove phosphates, etc. as a stabilizer added to the solution of the organic peracid) to give the aimed resin. Preferably 0.8W2.5g equivalents, based on one g equivalent allyl groups in the allyl etherified novolak resin, organic peracid is used.
    COPYRIGHT: (C)1984,JPO&Japio

    Abstract translation: 目的：为了获得用于密封绝缘材料和半导体几乎没有残留卤素的酚醛清漆环氧树脂，可以通过用有机过酸将液态烯丙基醚化的酚醛清漆树脂环氧化。 构成：烯丙醚醚化酚醛清漆树脂，例如 通过在苯酚或甲酚和福尔马林中合成酚醛清漆树脂而获得的树脂，并使所得的酚醛清漆树脂与烯丙基卤在碱金属氢氧化物的存在下反应而获得。 己烷，并与有机过酸，优选过乙酸的溶液反应，优选在40-70℃的反应温度。 对所得到的溶液进行除去溶剂和有机酸，并且如果需要，将脱盐（作为添加到有机过酸溶液中的稳定剂的磷酸盐等）除去，得到目标树脂。 优选0.8-2.5g当量，基于烯丙基醚化酚醛清漆树脂中的1g当量烯丙基，使用有机过酸。

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