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    • 2. 发明授权
    • Method for the production of polytetramethylene ether glycol
    • 生产聚四亚甲基醚二醇的方法
    • US5393866A
    • 1995-02-28
    • US149779
    • 1993-11-10
    • Nobuyuki MuraiMasayuki ShiratoHiroshi TakeoHidetoshi Tanaka
    • Nobuyuki MuraiMasayuki ShiratoHiroshi TakeoHidetoshi Tanaka
    • C08G65/20C08G65/26C08G65/324C08G59/68C07C43/02C08G65/04
    • C08G65/20C08G65/2678C08G65/2684C08G65/324
    • A method for the production of polytetramethylene ether glycol wherein polymerization of tetrahydrofuran in the presence of fluorosulfonic acid is followed by hydrolysis of the resulting polymer, characterized by(1) using the fluorosulfonic acid at 0.007-0.3 molar equivalents with respect to the tetrahydrofuran;(2) using in combination therewith fuming sulfuric acid which contains free sulfur trioxide at 0.05-1.0 molar equivalent with respect to the fluorosulfonic acid; and(3) adding said fuming sulfuric acid to the tetrahydrofuran prior to adding the fluorosulfonic acid thereto.According to the method, high quality polytetramethylene ether glycol with a low fluorine content may be obtained at a high yield without lowering the polymerization temperature. For example, PTMG may be obtained with 3 or fewer, and preferably 2 or fewer terminal fluorines per 2,000 termini of the resulting PTMG. As a result, when the resulting PTMG is used as a starting material for elastomers, it is possible to easily obtain a high molecular weight polymer with excellent heat resistance.
    • 一种生产聚四亚甲基醚二醇的方法,其中在氟磺酸存在下聚合四氢呋喃,然后水解所得聚合物,其特征在于(1)使用相对于四氢呋喃0.007-0.3摩尔当量的氟磺酸; (2)与含有相对于氟磺酸的0.05-1.0摩尔当量的游离三氧化硫的发烟硫酸组合使用; 和(3)在向其中加入氟磺酸之前将所述发烟硫酸加入到四氢呋喃中。 根据该方法,可以在不降低聚合温度的情况下以高产率获得低含氟量的高品质聚四亚甲基醚二醇。 例如,PTMG可以获得3个以下,优选2个以下的末端荧光,每2 000个终点产生的PTMG。 结果,当所得到的PTMG用作弹性体的起始材料时,可以容易地获得具有优异耐热性的高分子量聚合物。
    • 4. 发明授权
    • Writing board ink composition
    • 书写板油墨组成
    • US5318617A
    • 1994-06-07
    • US38474
    • 1993-03-29
    • Toshiyuki NagasawaNobuyuki MuraiKazuo Goda
    • Toshiyuki NagasawaNobuyuki MuraiKazuo Goda
    • C09D11/16C09D11/17
    • C09D11/17
    • A writing board ink composition comprises a medium formed of a lower alcohol solvent which contains an alcohol-soluble polymer, a scraping (erasing) agent, a surfactant and a diketopyrrolopyrrole pigment having a median Stokes diameter (ultrafine particle size) of not more than 0.2 .mu.m and represented by the following formula ##STR1## R.sup.1 and R.sup.2 independently represent an unsubstituted phenyl or naphthyl group of a non-water-solubilizing substituent substituted phenyl or naphthyl group, and R.sup.3 and R.sup.4 independently represent hydrogen or a non-water-solubilizing substituent. The writing board ink composition remains stable for a long time while in pens even when the resin content (alcohol-soluble polymer) is such that unclear writing and scrapability reduction (loss of scrapability or erasability) can be avoided, since the pigment of ultrafine particle size is fast to lower alcohol solvents.
    • 书写用油墨组合物包含由含有醇溶性聚合物的低级醇溶剂,刮擦(擦除)剂,表面活性剂和二仲吡咯并吡咯颜料形成的介质,所述颜料的中等斯托克斯直径(超微粒径)不大于0.2 并且由下式表示:其中R 1和R 2独立地表示非水溶性取代基的取代的苯基或萘基的未取代的苯基或萘基,R 3和R 4独立地表示氢或非 - 水溶性取代基。 即使当树脂含量(醇溶性聚合物)具有不清楚的书写和可刮除性降低(可刮除性或可擦除性的损失))时,书写用墨水组合物长时间保持稳定,而由于超细颗粒的颜料 大小很快降低酒精溶剂。
    • 9. 发明授权
    • Process for preparing diacetoxybutene
    • 制备二乙酰氧基丁烯的方法
    • US5429721A
    • 1995-07-04
    • US245663
    • 1994-05-18
    • Hiroaki KandoriNobuyuki Murai
    • Hiroaki KandoriNobuyuki Murai
    • B01J23/44C07B61/00C07C67/055C07C67/54C07C69/16B01D3/10C07C69/02
    • C07C67/54C07C67/055
    • A process for preparing diacetoxybutene, including:reacting butadiene, acetic acid and oxygen in the presence of a palladium-based catalyst;feeding continuously the resulting reaction product into a first distillation tower;feeding continuously a withdrawn bottoms withdrawn from the first distillation tower into a second distillation tower;withdrawing bottoms containing high boiling point materials from the bottom of the second distillation tower, so that the content of the high boiling point materials in the bottoms of the second distillation tower is not more than 20 wt %;feeding continuously the withdrawn bottoms into a thin-film evaporator whose internal pressure is kept lower than the bottom pressure of the second distillation tower to carry out evaporation treatment; andrecycling the evaporated materials mainly containing diacetoxybutene into the second distillation tower.
    • 一种制备二乙酰氧基丁烯的方法,包括:在钯基催化剂存在下使丁二烯,乙酸和氧反应; 将所得反应产物连续进料到第一蒸馏塔中; 将从第一蒸馏塔排出的回收塔底馏分连续进料到第二蒸馏塔中; 从第二蒸馏塔的底部排出含有高沸点物质的塔底物,使得第二蒸馏塔底部的高沸点物质的含量不大于20wt%; 将取出的底部物料连续进入薄膜蒸发器,其内部压力保持低于第二蒸馏塔的底部压力以进行蒸发处理; 并将主要含有二乙酰氧基丁烯的蒸发材料回收到第二蒸馏塔中。