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    • 4. 发明授权
    • Production of liquid ortho-phthalic acid and its conversion to high
purity phthalic anhydride
    • 液态邻苯二甲酸的生产及其转化为高纯度邻苯二甲酸酐
    • US4215054A
    • 1980-07-29
    • US70827
    • 1979-08-29
    • Hobe SchroederGeorge E. KuhlmannSydney G. HorsfieldDavid A. Palmer
    • Hobe SchroederGeorge E. KuhlmannSydney G. HorsfieldDavid A. Palmer
    • C07C51/265C07C51/56C07D307/89
    • C07C51/265C07C51/56
    • Phthalic anhydride of commercially acceptable quality can be recovered from the neat catalytic oxidation of liquid o-xylene with air in the presence of the catalysis system provided by cobalt, manganese and bromine conducted in a single step and in the presence of a small amount of benzoic acid to make miscible liquid o-phthalic acid and liquid oxylene conducted in a single step to an 80 to 90 mole percent yield of o-phthalic acid provided the resulting liquid oxidation effluent is subjected to rapid dehydration of o-phthalic acid to its anhydride and rapid evaporation of the anhydride, water and compounds boiling between water and said anhydride which evaporation entrains phthalide in the vapor mixture followed by contact of the vapor mixture with Pd/C and introducing the vapor mixture into a fractionating system whose reflux liquid is inert, boils at a temperature below the boiling temperature of phthalic anhydride and is a solvent therefor at a temperature below the freezing temperature of said anhydride whereby impure liquid anhydride is withdrawn as water-free liquid and charged to a step of heating with alkali metal hydroxide to remove phthalide and then fractionated to remove benzoic acid as a first fraction, high purity phthalic anhydride as a second fraction and materials boiling higher than the anhydride as a liquid third fraction.
    • 可在商业上可接受的质量的邻苯二甲酸酐在由钴,锰和溴提供的催化体系存在下,在单一步骤中并在少量苯甲酸存在下,从液体邻二甲苯的纯催化氧化中回收 酸使得可混合的邻苯二甲酸和液体氧化烯在一个步骤中进行至80至90摩尔%的邻苯二甲酸产率,条件是所得的液体氧化流出物经其邻苯二甲酸快速脱水至其酸酐, 酸酐,水和水和所述酸酐之间沸腾的化合物的蒸发迅速蒸发,蒸发在蒸气混合物中引入苯并呋喃,随后蒸气混合物与Pd / C接触,并将蒸汽混合物引入回流液体惰性的分馏系统中 在低于邻苯二甲酸酐的沸点温度的温度下,在低于冷冻温度的温度下为其溶剂 所述酸酐的所述酐,由此使不纯的液体酸酐作为无水液体排出,并加入到用碱金属氢氧化物加热以除去苯酞的步骤,然后分馏以除去作为第一级分的苯甲酸,作为第二馏分的高纯度邻苯二甲酸酐, 沸点高于酸酐的物质作为液体第三级分。
    • 10. 发明授权
    • Preparation of phthalic acid by single step continuous air oxidation of
liquid ortho-xylene
    • 通过单步连续空气氧化液相邻二甲苯制备邻苯二甲酸
    • US4211881A
    • 1980-07-08
    • US961763
    • 1978-11-17
    • Sydney G. HorsfieldGeorge E. KuhlmannAlan G. Bemis
    • Sydney G. HorsfieldGeorge E. KuhlmannAlan G. Bemis
    • C07C51/265C07C51/33
    • C07C51/265
    • This invention relates to the neat air oxidation of liquid o-xylene in a continuous manner in a single step to overcome the limited conversion of the process of British Patent Specification No. 856,245 or of the process of U.S. Pat. No. 3,920,735. More specifically this invention overcomes the limited conversion of o-xylene by its single step air oxidation in the presence of catalysis provided by ions of cobalt, manganese and bromine not only by maintaining the proper relationship of temperature, pressure and free water concentration in the reaction mixture to minimize the conversion of o-phthalic acid to its intramolecular anhydride but also by conducting the oxidation in the presence of small amounts of acetic or benzoic acid to make miscible the otherwise immiscible liquid phases of liquid o-xylene and liquid o-phthalic acid containing components of catalysis and free liquid water.
    • 本发明涉及在一个步骤中以连续方式连续地液体邻二甲苯的纯空气氧化,以克服英国专利说明书856,245或美国专利第856,245号的方法的有限转化。 第3,920,735号。 更具体地,本发明克服了在由钴,锰和溴离子提供的催化剂存在下,通过其单步空气氧化对邻二甲苯的有限转化,不仅通过保持反应中温度,压力和游离水浓度的适当关系 使邻苯二甲酸转化为其分子内酸酐的最小化,还可以在少量乙酸或苯甲酸的存在下进行氧化,使混溶的液体邻二甲苯和液体邻苯二甲酸的其它不混溶液相 含有催化成分和游离液态水。