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    • 1. 发明授权
    • Process for producing cellulose acetate
    • 生产乙酸纤维素的方法
    • US4439605A
    • 1984-03-27
    • US433615
    • 1982-10-12
    • Hideo YabuneYoshiyuki IkemotoYounosuke KatoManabu Uchida
    • Hideo YabuneYoshiyuki IkemotoYounosuke KatoManabu Uchida
    • C08B3/06C08B3/24
    • C08B3/24C08B3/06
    • A process for producing cellulose diacetate is disclosed which comprises the steps of:(a) pretreating and activating 100 parts by weight of cellulose, adding a mixture of 200 to 400 parts of acetic anhydride, 0 to 350 parts of glacial acetic acid, and 0.5 to 5 parts of acid catalyst, heating the reactants to a temperature from 50.degree. C. to 85.degree. C. at approximately a constant rate, maintaining this temperature for 3 to 20 minutes, thereby acetylating cellulose to form primary cellulose acetate;(b) neutralizing the acid catalyst in the reaction mixture containing primary cellulose acetate obtained in step (a), introducing steam under pressure into the system to change the temperature of the system to 125.degree. C. to 170.degree. C., and maintaining this temperature for 30 minutes to 6 hours, thereby hydrolyzing the primary cellulose acetate to accomplish ripening; and(c) flashing the ripened reaction mixture at a temperature of 125.degree. C. to 170.degree. C. by discharging same to the ambient atmosphere, recovering by condensation the gas generated during flashing having an acetic acid/water weight ratio of 70-80/30-20, and simultaneously cooling the remaining liquid reaction mixture to about 100.degree. C., thereby substantially stopping the hydrolysis reaction.
    • 公开了一种制备纤维素二乙酸酯的方法,其包括以下步骤:(a)预处理和活化100重量份的纤维素,加入200-400份乙酸酐,0-350份冰乙酸和0.5份 至5份酸催化剂,以大约恒定速率将反应物加热至50℃至85℃的温度,将该温度保持3至20分钟,由此乙酰化纤维素以形成乙酸纤维素; (b)中和在步骤(a)中获得的含有初级纤维素乙酸酯的反应混合物中的酸催化剂,将压力下的蒸汽引入体系中以将体系的温度改变至125℃至170℃,并保持该 温度30分钟至6小时,从而水解初级纤维素乙酸酯以达到熟化; 和(c)将熟化的反应混合物在125℃至170℃的温度下闪蒸,通过将其排放到环境大气中,通过冷凝回收,在闪蒸期间产生的气体具有70-80的乙酸/水重量比 / 30-20,同时将剩余的液体反应混合物冷却至约100℃,从而基本上停止水解反应。
    • 2. 发明授权
    • Process for producing cellulose diacetate having improved resistance to
delustering phenomenon in hot water
    • 具有改善的耐热消光现象的纤维素二乙酸酯的制造方法
    • US4269972A
    • 1981-05-26
    • US047469
    • 1979-06-11
    • Hideo YabuneYoshiyuki Ikemoto
    • Hideo YabuneYoshiyuki Ikemoto
    • C08B3/06
    • C08B3/06
    • Cellulose diacetate having improved resistance to delustering in hot water is produced by acetylation cellulose in the presence of a catalyst and then hydrolyzing (or ripening) the product to form secondary cellulose acetate; wherein the catalyst in the acetylated mixture is completely neutralized before about the middle of the hydrolysis reaction at the latest and thereafter hydrolysis is carried out at a temperature of about 110.degree. to 120.degree. C. while maintaining the concentration of acetic acid in the reaction mixture at about 67 to 78% by weight based on the total weight of the acetic acid and water, the relation between the hydrolysis temperature and the concentration of acetic acid being defined by the area between and including points A, B, C and D in FIG. 2.
    • 乙酰化纤维素在催化剂存在下产生具有改善的热水消光耐性的纤维素二乙酸酯,然后水解(或熟化)该产物以形成乙酸纤维素; 其中乙酰化混合物中的催化剂最近在水解反应中间完全中和,然后水解在约110-120℃的温度下进行,同时保持反应混合物中乙酸的浓度 以乙酸和水的总重量计约67至78重量%,水解温度与乙酸浓度之间的关系由图3中的点A,B,C和D之间的面积和包括点A,B,C和D之间的面积 。 2。
    • 4. 发明授权
    • Method for producing acetylated pyroxylin
    • 生产乙酰化pyroxylin的方法
    • US06417345B1
    • 2002-07-09
    • US09414832
    • 1999-10-08
    • Tokuji TanakaNoboru KameiHideo Yabune
    • Tokuji TanakaNoboru KameiHideo Yabune
    • C08B502
    • C08B7/00
    • The invention provides a method for producing acetylated pyroxylin with safety yet at low cost, using inexpensive water-wetted pyroxylin rather than expensive alcohol-wetted pyroxylin. The acetylated pyroxylin is produced by dehydrating the water-wetted pyroxylin in the presence of a nonalcoholic non-solvent for pyroxylin, and then permitting an acetylating agent to act on the dehydrated pyroxylin. According to the first dehydration process, the water-wetted pyroxylin is dispersed in a dispersing medium comprising a nonalcoholic non-solvent for pyroxylin, and then dehydrated by distillation. According to the second dehydration process, a replacing agent comprising a nonalcoholic non-solvent for pyroxylin is added to the water-wetted pyroxylin, and the wetted pyroxylin is then dehydrated by filtration. With either one of these processes, the water-wetted pyroxylin can be dehydrated with safety.
    • 本发明提供了一种使用廉价的水润湿菌素而不是昂贵的酒精润湿的pyroxylin以低成本安全地生产乙酰化pyroxylin的方法。 乙酰化的pyroxylin是通过在用于pyroxylin的非醇非溶剂的存在下使水润湿的pyroxylin脱水,然后允许乙酰化剂作用于脱水的pyroxylin而产生的。 根据第一脱水方法,将水润的富霉素分散在包含用于pyroxylin的非醇非溶剂的分散介质中,然后通过蒸馏脱水。 根据第二脱水方法,将含有不溶性焦油石蜡的非溶剂的替代剂加入到水润的辉石中,然后通过过滤将湿润的富霉素脱水。 使用这些方法之一,可以安全地脱水水润的pyroxylin。
    • 5. 发明授权
    • Cellulose ester resin composition
    • 纤维素酯树脂组合物
    • US4209340A
    • 1980-06-24
    • US881628
    • 1978-02-27
    • Hideo YabuneMasami Nambu
    • Hideo YabuneMasami Nambu
    • C08L1/00C08K5/524C08K5/527C08L1/10
    • C08K5/524C08K5/52C08K5/527
    • A resin composition comprising an organic acid ester of cellulose, as a resin component, and at least one member selected from organic phosphite compounds having the formulae (i) and (ii): ##STR1## wherein R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5 and R.sub.6, which can be the same or different, each is hydrogen, alkyl, aryl, alkylaryl, arylalkyl, alkoxyaryl, alkoxyalkyl, polyalkoxyalkyl, polyalkoxyaryl or polyaryloxyalkyl groups, with the proviso that one of R.sub.1 and R.sub.2 and one or two of R.sub.3, R.sub.4, R.sub.5 and R.sub.6 can be hydrogen, and R.sub.1 ' and R.sub.2 ', which can be the same or different, each is hydrogen or alkyl, aryl, alkoxyalkyl, aryloxyalkyl, alkoxyaryl, arylalkyl, alkylaryl, polyaryloxyalkyl, polyalkoxyalkyl and polyalkoxyaryl groups, and n is a number of at least 1, preferably 1 to 5.
    • (i)和(ii)所示的有机亚磷酸酯化合物中的至少一种:作为树脂成分的纤维素有机酸酯和选自有机亚磷酸酯化合物中的至少一种的树脂组合物, 其中可以相同或不同的R 1,R 2,R 3,R 4,R 5和R 6各自为氢,烷基,芳基,烷基芳基,芳基烷基,烷氧基芳基,烷氧基烷基,聚烷氧基烷基,聚烷氧基芳基或聚芳氧基烷基,条件是 R 1和R 2以及R 3,R 4,R 5和R 6中的一个或两个可以是氢,并且可以相同或不同的R 1'和R 2'各自为氢或烷基,芳基,烷氧基烷基,芳氧基烷基,烷氧基芳基,芳基烷基, 烷芳基,聚芳氧基烷基,聚烷氧基烷基和聚烷氧基芳基,n为至少1,优选1至5的数。