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    • 3. 发明授权
    • Process for removal of high molecular weight impurities in the
manufacture of purified terephthalic acid
    • 在制备纯对苯二甲酸中除去高分子量杂质的方法
    • US4782181A
    • 1988-11-01
    • US58142
    • 1987-06-04
    • David E. James
    • David E. James
    • C07C51/487C07C51/42
    • C07C51/487
    • A process for producing fiber grade terephthalic acid is disclosed. In this process impurities having high molecular weight are eliminated by hydrogenation comprising the following steps: (a) treating an aqueous solution containing at least about 1 percent of said impure terephthalic acid with hydrogen at a temperature in the range of about 300.degree. F. to about 450.degree. F. and at a pressure sufficient to maintain the solution in the liquid phase in the presence of a supported or unsupported metallic Group VIII noble metal catalyst wherein both the metal and support components are insoluble in the solution at the temperature and at a hydrogen partial pressure of from about 30 to about 300 pounds per square inch; (b) separating the treated solution from the catalyst; (c) crystallizing terephthalic acid from the separated solution while retaining impurities and the reduced aromatic compounds dissolved in the resulting mother liquor at a temperature in the range of about 100.degree. F. to about 450.degree. F.; and (d) separating the mother liquor as a liquid phase containing dissolved impurities and reduction products from said crystals while continuing to maintain a temperature in the range of about 100.degree. F. to about 450.degree. F. whereby purified crystals of fiber grade terephthalic acid are recovered. Purified terephthalic acid is useful as a starting material in the manufacture of polyethylene terephthalate which is the principal polymer for polyester fibers, films, and resins for bottles.
    • 公开了一种生产纤维级对苯二甲酸的方法。 在该方法中,通过氢化除去具有高分子量的杂质,包括以下步骤:(a)在约300°F的温度范围内用氢处理含有至少约1%的所述不纯对苯二甲酸的水溶液至 在足够的压力下,在负载或未负载的金属VIII族贵金属催化剂存在下将溶液保持在液相中,其中金属和载体组分在温度下不溶于溶液,并且在 氢分压为约30至约300磅/平方英寸; (b)将处理过的溶液与催化剂分离; (c)从分离的溶液中结晶对苯二甲酸,同时保留杂质和溶解在所得母液中的还原芳族化合物在约100°F至约450°F的温度范围内; 和(d)将母液从含有溶解的杂质和还原产物的液相中分离出来,同时继续保持在约100°F至约450°F范围内的温度,从而将纤维级对苯二甲酸 被收回。 纯化的对苯二甲酸可用作制造聚对苯二甲酸乙二醇酯的原料,聚对苯二甲酸乙二醇酯是聚酯纤维,膜和树脂树脂的主要聚合物。
    • 9. 发明授权
    • Purification of crude terephthalic acid
    • 纯对苯二甲酸粗品
    • US4892972A
    • 1990-01-09
    • US344657
    • 1989-04-27
    • Hobe SchroederDavid E. James
    • Hobe SchroederDavid E. James
    • C07C51/487
    • C07C51/487
    • Aqueous solutions of crude terephthalic acid are purified by hydrogenation in the presence of plural noble metal catalysts in separate layers. Initially, the solution to be purified is passed through a layer of ruthenium-on-carbon catalyst, rhodium-on-carbon catalyst, or platinum-on-carbon catalyst, and thereafter through a layer of palladium-on-carbon catalyst. Optionally, the purified aqueous terephthalic acid solution can be treated further to decrease the 4-carboxybenzaldehyde content thereof by passing it through a layer of rhodium-on-carbon catalyst downstream from the palladium-on-carbon catalyst layer.
    • 在多层贵金属催化剂存在下,通过氢化纯化粗对苯二甲酸的水溶液。 最初,待纯化的溶液通过一层碳酸钌催化剂,铑 - 碳催化剂或铂 - 碳催化剂,然后通过一层钯 - 碳催化剂。 任选地,可以进一步处理纯化的对苯二甲酸水溶液,以使其通过使其通过碳 - 钯催化剂层下游的铑 - 碳催化剂层来降低其4-羧基苯甲醛含量。
    • 10. 发明授权
    • Process for preparation of anthraquinones and fluorenones
    • 制备蒽醌和芴酮的方法
    • US4822527A
    • 1989-04-18
    • US134839
    • 1987-12-14
    • David E. JamesNeal R. Nowicki
    • David E. JamesNeal R. Nowicki
    • C07C50/18C07C45/00
    • C07C50/18Y02P20/584
    • A process is disclosed for producing cyclized aromatic compounds by the liquid-phase air oxidation of 2-methyl-substituted biphenyls and diphenylmethanes in an acetic acid medium in the presence of a cobalt-manganese-bromine catalyst or a zirconium-cobalt-manganese-bromine catalyst wherein the mole ratio of cobalt-to-manganese is about 1.0:0.1 to about 1.0:10.0 and the ratio of zirconium-to-cobalt is about 0.005:1.0 to about 0.20:1.0, and mole ratio of bromine to total metals of said cobalt-manganese-bromine catalyst or zirconium-cobalt-manganese-bromine catalyst is from about 0.2:1.0 to about 20.0:1.0, which process comprises conducting the reaction in a batch process at a temperature of from 75.degree. C. to about 250.degree. C. at a pressure of from 1 to 100 atmospheres, or continuously in two stages comprising a first-stage reaction at a temperature of about 75.degree. C. to about 200.degree. C. and a second-stage reaction at a temperature of about 150.degree. C. to about 250.degree. C. and recycling the cobalt-manganese catalyst or the zircnium-cobalt-manganese catalyst by oxalate precipitation of the catalyst at temperatures of about 110.degree. C. to about 200.degree. C. prior to the separation of mother liquor and using about 0.25 to about 2.5 moles of oxalic acid per mole of cobalt and manganese or mole of zirconium-cobalt-manganese and continuously recycling the recovered catalyst metals to the oxidation stages. The products of this novel process, anthraquinones and fluorenones, are useful for the manufacture of dyestuffs and pharmaceuticals.
    • 公开了在钴锰溴催化剂或锆 - 钴 - 锰 - 溴存在下,通过在乙酸介质中通过2-甲基取代的联苯和二苯基甲烷的液相空气氧化来生产环化芳族化合物的方法 催化剂,其中钴与锰的摩尔比为约1.0:0.1至约1.0:10.0,锆与钴的摩尔比为约0.005:1.0至约0.20:1.0,溴与总金属的摩尔比为 所述钴 - 锰 - 溴催化剂或锆 - 钴 - 锰 - 溴催化剂的量为约0.2:1.0至约20.0:1.0,该方法包括在75℃至约250℃的间歇过程中进行反应 在1〜100个大气压的压力下,或者在约75℃至约200℃的温度下包括第一阶段反应的两个阶段的连续两个阶段,以及在约 150℃至约250℃并回收 钴锰催化剂或锆 - 钴 - 锰催化剂,在母液分离之前,在约110℃至约200℃的温度下草酸盐沉淀催化剂,并使用约0.25至约2.5摩尔的草酸 每摩尔钴和锰或摩尔的锆 - 钴 - 锰,并将回收的催化剂金属连续循环到氧化阶段。 该新方法的产物,蒽醌和芴酮可用于制造染料和药物。