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    Process for the preparation of naphthalene-1,4,5,8-tetracarboxylic acid
    1.
    发明授权
    Process for the preparation of naphthalene-1,4,5,8-tetracarboxylic acid 失效
    萘-1,4,5,8-四羧酸的制备方法

    公开(公告)号：US4097492A

    公开(公告)日：1978-06-27

    申请号：US683039

    申请日：1976-05-04

    Applicant: Freimund Rohrscheid

    Inventor： Freimund Rohrscheid

    IPC: C07C51/31 ,  C07D311/02 ,  C07C51/33

    CPC classification number: C07C51/316

    Abstract: Naphthalene-1,4,5,8-tetracarboxylic acid and typical derivative(s) thereof is (are) prepared by oxidation of periacenaphthindenones of the formula ##STR1## where R is H or lower alkyl, in a lower aliphatic carboxylic acid with nitric acid, optionally using also oxygen, in the presence of oxidation catalysts at temperatures above about 100.degree. C; the reaction product being worked up in known manner. Naphthalene-1,4,5,8-tetracarboxylic acid is an important preliminary product for the manufacture of dyestuffs.

    Abstract translation: 萘-1,4,5,8-四羧酸及其典型的衍生物通过在低级脂族羧酸与硝酸中氧化式（IMAGE）其中R是H或低级烷基的苊萘醌来制备 酸，任选地还使用氧，在氧化催化剂存在下，在高于约100℃的温度下; 反应产物以已知的方式处理。 萘-1,4,5,8-四羧酸是制造染料的重要初步产品。

    Bismuth enhanced activity of transition metal-bromine catalysis of di- and tri-methyl benzene oxidation in liquid phase
    2.
    发明授权
    Bismuth enhanced activity of transition metal-bromine catalysis of di- and tri-methyl benzene oxidation in liquid phase 失效
    铋提高了液相中二 - 和三 - 甲苯氧化过渡金属 - 溴催化活性

    公开(公告)号：US3931304A

    公开(公告)日：1976-01-06

    申请号：US362463

    申请日：1973-05-21

    Applicant: Gene L. Wampfler

    Inventor： Gene L. Wampfler

    IPC: C07C51/265 ,  C07C51/33

    CPC classification number: C07C51/265

    Abstract: Addition of non-transitional bismuth ion to oxidation catalysis provided by heavy, transition metal-bromine ion combination containing both cobalt and manganese ions uniquely increases catalytic activity of said combination for converting ortho substituted methyl groups to corresponding carboxylic acid groups on benzene nucleus by a factor much greater than by the addition of equivalent amount of such high catalytically active heavy, transition metal as cobalt and manganese. Such greater catalytic activity is manifested by longer sustained initial rapid rate of oxygen consumption and higher o-dicarboxybenzene yield.

    Abstract translation: 将非过渡性铋离子添加到含有钴和锰离子的重的过渡金属 - 溴离子组合提供的氧化催化中，独特地提高了所述组合的催化活性，以将邻位取代的甲基转化成相对于苯核上的相应羧酸基团 远远大于加入等量的这种高催化活性的重金属，过渡金属如钴和锰。 这种更大的催化活性通过更长的持续的初始快速氧消耗速率和较高的邻二羧基苯产率来表现。

    Purification of recirculated stream for isophthalic acid production
    4.
    发明授权
    Purification of recirculated stream for isophthalic acid production 失效
    用于间苯二甲酸生产的再循环流的净化

    公开(公告)号：US3919306A

    公开(公告)日：1975-11-11

    申请号：US25982972

    申请日：1972-06-05

    Applicant: ATLANTIC RICHFIELD CO

    Inventor： JOHNSON CARL E ,  BAKER ALAN D

    IPC: C07C51/265 ,  C07C51/42 ,  C07C51/33

    CPC classification number: C07C51/265 ,  C07C51/42 ,  Y02P20/582 ,  C07C63/24

    Abstract: Technical grades of meta xylene employed in manufacturing isophthalic acid generally contain very small amounts of ortho and/or para xylene, leading to the formation of troublesome amounts of orthophthalic acid and terephthalic acid, which are troublesome in the cayalytic oxidation of meta xylene to isophthalic acid in an oxidative reaction zone. The recirculated acetic acid solvent tends to accumulate contaminants such as orthophthalic acid, terephthalic acid, and related impurities. There is the possibility of contamination of the isophthalic acid product by terephthalic acid, benzoic acid, and/or other impurities. Even small amounts of orthophthalic acid are extremely harmful because orthophthalic acid is a catalyst poison. Any troublesome accumulation of contaminants is prevented by the unique combination of steps for purification of the recycled stream. All of the orthophthalic acid (catalyst poison) is removed as the sodium salt in an aqueous filtrate after a precipitate comprising cobalt carbonate has been filtered from a mixture of aqueous sodium carbonate and a stripped bottoms solution. Cobalt acetate is regenerated from the cobalt carbonate precipitate by reaction with a portion of the overhead stream from the flash distillation of the stream from which the isophthalic acid has been removed. Water is desirably removed from the acetic acid prior to its recirculation to the oxidative reaction zone. Only small proportions of make up cobalt acetate and/or make up acetic acid must be added to the recirculated solution because of the high efficiency of the purification of the acetic acid solvent and the high efficiency of the purification of the cobalt acetate catalyst and the satisfactory removal of orthophthalic acid related catalyst poisons from the purified cobalt catalyst.

    Abstract translation: 用于制造间苯二甲酸的间二甲苯的技术等级通常含有非常少量的邻位和/或对二甲苯，导致形成麻烦的邻苯二甲酸和对苯二甲酸，这在间二甲苯到间苯二甲酸的催化氧化中是麻烦的 在氧化反应区。 再循环的乙酸溶剂易于积聚污染物如邻苯二甲酸，对苯二甲酸和相关杂质。 可以通过对苯二甲酸，苯甲酸和/或其他杂质污染间苯二甲酸产物。 即使少量的邻苯二甲酸也是非常有害的，因为邻苯二甲酸是一种催化剂毒物。 污染物的任何麻烦的积累通过用于净化再循环流的步骤的独特组合来防止。 在从碳酸钠水溶液和汽提的底部溶液的混合物中过滤包含碳酸钴的沉淀物之后，将所有邻苯二甲酸（催化剂毒物）作为钠盐在水性滤液中除去。 通过与已经除去间苯二甲酸的物流的闪蒸的一部分顶部物流反应，从碳酸钴沉淀物中再生乙酸钴。 在再循环到氧化反应区之前，希望从乙酸中除去水。 由于乙酸溶剂的纯化效率高，乙酸钴催化剂的纯化效率高，所以必须将少量的乙酸钴和/或乙酸组成添加到再循环溶液中 从纯化的钴催化剂中除去邻苯二甲酸的催化剂毒物。

    Method of preparing p-nitrobenzoic acid
    7.
    发明授权
    Method of preparing p-nitrobenzoic acid 失效
    对硝基苯甲酸的制备方法

    公开(公告)号：US4007223A

    公开(公告)日：1977-02-08

    申请号：US535862

    申请日：1974-12-23

    Applicant: Marcel Feld ,  Hermann Richtzenhain

    Inventor： Marcel Feld ,  Hermann Richtzenhain

    IPC: C07B61/00 ,  B01J27/00 ,  B01J31/00 ,  C07C67/00 ,  C07C201/00 ,  C07C201/12 ,  C07C205/57 ,  C07C205/59 ,  C07C51/33

    CPC classification number: C07C205/57 ,  C07C201/12

    Abstract: Process of preparing a not discolored p-nitrobenzoic acid by oxidation of p-nitrotoluene with oxygen, which comprises contacting the oxygen with the p-nitrotoluene in an acetic acid reaction medium and in the presence of a cobalt-containing and bromine-containing catalyst at a temperature of 80.degree. to 150.degree. C. The cobalt is present as a cobalt salt in the amount of 0.01 to 0.1 moles per mole of p-nitrotoluene, and the amount of acetic acid is 3 to 15 moles per mole p-nitrotoluene.

    Abstract translation: 通过用氧氧化对硝基甲苯来制备未变色的对硝基苯甲酸的方法，其包括使氧与对硝基甲苯在乙酸反应介质中并在含钴和溴的催化剂存在下接触 钴的存在量为每摩尔对硝基甲苯0.01至0.1摩尔的钴盐，每摩尔对硝基甲苯的乙酸量为3至15摩尔。

    Processes for the continuous production of aromatic carboxylic acids by oxidation with nitric acid of aromatic compounds containing oxidizable acyclic substituents
    8.
    发明授权
    Processes for the continuous production of aromatic carboxylic acids by oxidation with nitric acid of aromatic compounds containing oxidizable acyclic substituents 失效
    通过用含有可氧化的无环取代基的芳族化合物的硝酸氧化连续生产芳族羧酸的方法

    公开(公告)号：US3979448A

    公开(公告)日：1976-09-07

    申请号：US478395

    申请日：1974-06-11

    Applicant: Kurt Handrick ,  Anton Benning ,  Dietrich George ,  Jurgen Schlegel

    Inventor： Kurt Handrick ,  Anton Benning ,  Dietrich George ,  Jurgen Schlegel

    IPC: C07C63/00 ,  C07C51/00 ,  C07C51/275 ,  C07C67/00 ,  C07C205/24 ,  C07C205/57 ,  C07C51/33

    CPC classification number: C07C51/275 ,  C07C205/24 ,  C07C205/57

    Abstract: Processes for the continuous production of aromatic carboxylic acids by reaction of nitric acid with an aromatic compound having an oxidizable alkyl or alkoxyalkyl substitutent which comprise mixing the aromatic compound in the form of small droplets with a large volume of dilute nitric acid having a concentration between 2 and 14% by weight of nitric acid that is maintained at a superatmospheric pressure between 15 and 80 atmospheres and at a temperature between 160.degree. and 230.degree.C, which processes comprise continuously passing a reaction mixture consisting of the aromatic compound and the dilute nitric acid through a series of at least three consecutively arranged vertical reactor column in each of which the ratio of the weight of the reaction mixture containing the dilute nitric acid to the weight of the aromatic compound is continuously maintained at at least 50:1, the nitric acid concentration in each of the reactor column being continuously maintained at an originally preselected concentration by the addition of amounts of more-concentrated nitric acid while aliquot portions of the aromatic compound based upon the number of vertical reactor columns in the series are continuously introduced into each of the reactor columns, the reaction zones each being maintained at an optimal oxidation temperature between 160 and 230.degree.C for the aromatic compound that is being oxidized, and continuously passing the reaction mixture into a final reactor column that is maintained at a higher temperature than the preceding series of reactor columns, and continuously discharging the reaction mixture containing between 10 and 20% by weight of the aromatic carboxylic acid thus produced from the final reactor column.

    Abstract translation: 通过硝酸与具有可氧化烷基或烷氧基烷基取代基的芳族化合物的反应连续生产芳族羧酸的方法，其包括将小液滴形式的芳族化合物与大体积的浓度为2 和14重量％的硝酸，其保持在15至80个大气压之间的超大气压力和160-230℃的温度，该方法包括连续通过由芳族化合物和稀硝酸组成的反应混合物 通过一系列至少三个连续排列的立式反应器塔，其中含有稀硝酸的反应混合物的重量与芳族化合物的重量的比例连续保持在至少50:1，硝酸 每个反应器塔中的浓度连续保持在原来的预选中 通过加入较多浓度的硝酸的浓度，同时将基于该系列中的垂直反应器塔的数量的芳族化合物的等分试样部分连续引入每个反应器塔中，每个反应区保持在最佳状态 氧化温度在160〜230℃之间，待氧化的芳族化合物，并将反应混合物连续通入保持在比上一系列反应器塔高的温度的最终反应器塔中，并连续排出含有 10至20重量％的由最终反应器塔产生的芳族羧酸。

    Quality of phthalic acids improved by haloacetic acid
    10.
    发明授权
    Quality of phthalic acids improved by haloacetic acid 失效
    卤代乙酸改善邻苯二甲酸的质量

    公开(公告)号：US3947494A

    公开(公告)日：1976-03-30

    申请号：US316857

    申请日：1972-12-20

    Applicant: George E. Kuhlmann

    Inventor： George E. Kuhlmann

    IPC: C07C51/265 ,  C07C51/33

    CPC classification number: C07C51/265

    Abstract: Phthalic acids of improved quality are obtained direct from oxidation of xylenes with molecular oxygen in oxidation zone having small amounts of haloacetic acid present in liquid phase acetic acid solution of one or more heavy metal oxidation catalyst and bromide ion releasing bromine-containing compound. Particularly useful haloacetic acids are those having aqueous dissociation constant K.sub.A greater than 1.0 .times. 10.sup..sup.-3. Such quality improvement is manifested by decrease in carboxybenzaldehyde and toluic acid impurity contents and/or metal salt content.

    Abstract translation: 具有改善质量的邻苯二甲酸是直接从二氧化硅与分子氧的氧化反应获得的，该氧化区具有少量存在于一种或多种重金属氧化催化剂和溴离子释放含溴化合物的液相乙酸溶液中的卤代乙酸。 特别有用的卤代乙酸是具有大于1.0×10 -3的水解离常数KA的那些。 这种质量改善表现为羧基苯甲醛和甲苯酸杂质含量和/或金属盐含量的降低。

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