By-product recovery when oxidizing polymethylbenzenes to polycarboxylic
acids
    2.
    发明授权
    By-product recovery when oxidizing polymethylbenzenes to polycarboxylic acids 失效
    将聚甲基苯氧化成多元羧酸时的副产物回收

    公开(公告)号:US5118838A

    公开(公告)日:1992-06-02

    申请号:US722128

    申请日:1991-06-27

    IPC分类号: C07C51/47

    CPC分类号: C07C51/47

    摘要: Substantial proportions of methyl acetate and unreacted polymethylbenzene are recovered from the waste gas produced during the oxidation of a polymethylbenzene to its corresponding polycarboxylic acid by passing the waste gas, after being cooled for removal of water vapor, through at least one bed of activated carbon and subsequently desorbing the methyl acetate and polymethylbenzene from the bed by passing a desorbing medium, such as steam, through the bed. Preferably, the cooled stream is heated to a temperature of at least 21.degree. C. (70.degree. F.) prior to being passed into the bed of activated carbon.There is also disclosed an improved process for the oxidation of a polymethylbenzene to its corresponding aromatic polycarboxylic acid, which process comprises producing the polycarboxylic acid and waste gas comprising methyl acetate, water vapor, and unreacted polymethylbenzene and treating the waste gas according to the above method.

    摘要翻译: 在将聚甲基苯氧化成其相应的多元羧酸之前产生的废气中大量比例的乙酸甲酯和未反应的聚甲基苯通过使废气在冷却以除去水蒸汽后通过至少一个活性炭床和 然后通过使诸如蒸汽的解吸介质通过床来从床层解吸乙酸甲酯和聚甲基苯。 优选地,将冷却的流在进入活性炭床之前加热至至少21℃(70°F)的温度。 还公开了将聚甲基苯氧化成其相应的芳族多元羧酸的改进方法,该方法包括制备多元羧酸和包含乙酸甲酯,水蒸气和未反应的聚甲基苯的废气,并根据上述方法处理废气 。

    Low bromine content glacial acetic acid
    3.
    发明授权
    Low bromine content glacial acetic acid 失效
    低溴含量的冰醋酸

    公开(公告)号:US4278503A

    公开(公告)日:1981-07-14

    申请号:US106669

    申请日:1979-12-26

    IPC分类号: B01D3/14 C07C51/44 C07C51/16

    CPC分类号: B01D3/14 C07C51/44 Y02P20/582

    摘要: Excessive energy consumption of a combination of multi-fractionations and multi-distillations of concentrating aqueous acetic acid product of liquid phase oxidations, especially oxidation of liquid n-butane with oxygen gas while the butane is dissolved in liquid acetic acid containing a catalyst system comprising Co-Br or Co-Mn-Br, is avoided and an otherwise hard to remove bromo-ketone is readily removed by a combination of sequential steps of decompressing the oxidation reaction mixture to remove unreacted butane as well as gaseous products, heat treating the decompressed liquid at a temperature of from 150.degree. C. up to 200.degree. C. for from 15 up to 150 minutes, subjecting the heat treated liquid to fractionation while recycling to the rectification zone thereof an aqueous portion of low boiling impurities as a means for concentrating the acetic acid and thereafter further concentrating the acetic acid produced by continuous fractional crystallization.

    摘要翻译: 特别是在将丁烷溶解在含有Co的催化剂体系的液体乙酸中时,特别是用氧气氧化液体正丁烷的浓缩乙酸水溶液的多分馏和多馏分的多次分馏和多次蒸馏的过量能量消耗 -Br或Co-Mn-Br,并且通过将氧化反应混合物减压以除去未反应的丁烷以及气态产物的顺序步骤的组合容易地除去另外难以除去的溴酮,热处理减压的液体 在150℃至200℃的温度下15分钟至150分钟,对经热处理的液体进行分馏,同时将精馏区的低沸点杂质水溶液再循环至精馏区,作为浓缩 乙酸,然后进一步浓缩通过连续分级结晶产生的乙酸。

    Method and apparatus for controlling the manufacture of terephthalic
acid to control the level and variability of the contaminant content
and the optical density
    4.
    发明授权
    Method and apparatus for controlling the manufacture of terephthalic acid to control the level and variability of the contaminant content and the optical density 失效
    用于控制对苯二甲酸的制造的方法和装置,以控制污染物含量的水平和变异性以及光密度

    公开(公告)号:US4835307A

    公开(公告)日:1989-05-30

    申请号:US681227

    申请日:1984-12-13

    IPC分类号: B01J19/00 C07C51/265

    CPC分类号: B01J19/0006 C07C51/265

    摘要: The method and apparatus for manufacturing terephthalic acid (TA) are capable of producing TA having a closely controlled, desired amount of contaminant, 4-carboxy-benazldehyde (4-CBA), therein and/or a closely controlled optical density. In the method, a feed of para-xylene or similar feedstock mixed with catalyst components and solvent system is fed to a reactor stage comprising one or more reactors with oxygen for carrying out an exothermic oxidation reaction in the reactor stage, and an output slurry from the reactor stage is fed with oxygen to a first crystallizer of a crystallizing stage. The method comprises the steps of: determining empirical relationships between (1) the desired level of contaminant in the TA output product from the crystallizing stage and the oxygen uptake in the first crystallizer and (2) the oxygen uptake in the first crystallizer and the CO.sub.2 in the vent gas from the reactor stage; monitoring the CO.sub.2 in the vent gas from the reactor stage; and, adjusting operating variables of the reactor stage within minimum and maximum constraints thereof to adjust the reactor vent CO.sub.2 to a desired level.Also, the method includes the steps of: determining empirically a mathematical relationship between the oxygen in the vent gas from the reactor stage and the opticals or optical density of the TA output product; monitoring the oxygen in the vent gases; and, adjusting the air intake to the reactor stage until the oxygen in the reactor vent gas is at a desired level to provide TA output product with a desired optical density.The apparatus includes one or more reactors, one or more crystallizers, and control devices for carrying out the various steps of the method.

    摘要翻译: 用于制造对苯二甲酸(TA)的方法和装置能够产生其中具有严密控制的所需量的污染物的4-羧基 - 苯并三氢(4-CBA)和/或密度受控的光密度的TA。 在该方法中,将与催化剂组分和溶剂体系混合的对二甲苯或类似原料的进料进料到包含一个或多个反应器的反应器阶段,所述反应器具有氧气,用于在反应器阶段进行放热氧化反应, 将反应器级进料到氧气至结晶阶段的第一结晶器。 该方法包括以下步骤:确定(1)来自结晶阶段的TA输出产物中的污染物的期望水平与第一结晶器中的氧吸收之间的经验关系,以及(2)第一结晶器和CO 2中的氧吸收 在反应器阶段的排气中; 监测来自反应器阶段的排放气体中的二氧化碳; 并且将反应器级的操作变量调整到其最小和最大限制内以将反应器排气CO 2调整到期望的水平。 此外,该方法包括以下步骤:经验地确定来自反应器级的排放气体中的氧与TA输出产物的光学或光密度之间的数学关系; 监测排气中的氧气; 并且调节到反应器阶段的空气进入直到反应器排出气体中的氧气达到期望的水平,以提供具有期望的光密度的TA输出产物。 该装置包括一个或多个反应器,一个或多个结晶器和用于执行该方法的各个步骤的控制装置。

    Recycle of vaporized solvent in liquid phase oxidation of an alkyl
aromatic
    5.
    发明授权
    Recycle of vaporized solvent in liquid phase oxidation of an alkyl aromatic 失效
    在烷基芳族化合物的液相氧化中回收汽化溶剂

    公开(公告)号:US4777287A

    公开(公告)日:1988-10-11

    申请号:US665751

    申请日:1984-10-29

    CPC分类号: C07C51/265

    摘要: A method is disclosed for the continuous production of an aromatic carboxylic acid by the liquid phase, exothermic oxidation of an alkyl aromatic in a solvent in an oxidation reactor employing an overhead condenser system for condensation and recycle of vaporized solvent to the reactor, wherein the oxidation is performed at a relatively reduced temperature or pressure or at a relatively increased throughput of the alkyl aromatic without exceeding the elevation head between the condenser system and the reactor.

    摘要翻译: 公开了一种通过液相连续生产芳族羧酸的方法,在使用塔顶冷凝器系统的氧化反应器中的溶剂中的烷基芳族化合物的放热氧化,其中蒸发的溶剂冷凝并再循环到反应器中,其中氧化 在相对降低的温度或压力下或以相对增加的烷基芳族化合物的生产量进行,而不超过冷凝器系统和反应器之间的升降头。

    Process for removal and recycle of p-toluic acid from terephthalic acid
crystallizer solvent
    6.
    发明授权
    Process for removal and recycle of p-toluic acid from terephthalic acid crystallizer solvent 失效
    从对苯二甲酸结晶器溶剂中除去和循环对甲苯甲酸的方法

    公开(公告)号:US4500732A

    公开(公告)日:1985-02-19

    申请号:US532461

    申请日:1983-09-15

    IPC分类号: C07C51/48 C07C51/43

    CPC分类号: C07C51/48

    摘要: A process for the removal of para-toluic acid from purified terephthalic acid is disclosed. This process comprises extracting the para-toluic acid with paraxylene from the aqueous terephthalic acid-water phase and recycling the para-toluic acid and paraxylene to the paraxylene oxidation reactor. The process improves the overall yield of purified terephthalic acid recovered. Purified terephthalic acid is used as a basic raw material in the manufacture of polyester fibers and films.

    摘要翻译: 公开了从纯对苯二甲酸中除去对甲苯甲酸的方法。 该方法包括从对苯二甲酸 - 水相水相中用对二甲苯萃取对甲苯甲酸,并将对甲苯甲酸和对二甲苯再循环到对二甲苯氧化反应器中。 该方法提高了回收的纯对苯二甲酸的总产率。 纯化的对苯二甲酸用作制造聚酯纤维和薄膜的基本原料。

    Removal of bromobutanone from acetic acid
    7.
    发明授权
    Removal of bromobutanone from acetic acid 失效
    从乙酸中去除溴丁酮

    公开(公告)号:US4338464A

    公开(公告)日:1982-07-06

    申请号:US104088

    申请日:1979-12-17

    摘要: Acetic acid can be prepared in high conversions and selectively by the oxidation of liquid n-butane at temperatures of from 120.degree. C. up to 230.degree. C. in the presence of an acetic acid solution containing bromine ions in combination with ions of cobalt or cobalt and manganese. The debutanized effluent of such oxidation consists mainly of acetic acid and water but also contains esters and ketones boiling lower than acetic acid, some higher carbon content aliphatic acids and metal salts boiling higher than acetic acid and rather small amounts of 3-bromo-2-butanone which, although boiling higher than acetic acid, cannot be separated by simple distillation as can be the other non-acetic acid organic impurities. The present inventive technique for removal of said bromo-ketone has for its concept the use of a combination of cryogenic crystallization and removal of adhering mother liquor which can be practiced continuously in known apparatus devised for other fractional crystallizations.

    摘要翻译: 乙酸可以在高转化率和选择性地通过液体正丁烷的温度在120℃至230℃的温度下,在含有溴离子的乙酸溶液与钴离子的组合或 钴和锰。 这种氧化的脱锌废水主要由乙酸和水组成,但也含有比乙酸沸腾的酯和酮,一些较高碳含量的脂肪酸和沸点高于乙酸的金属盐,相当少量的3-溴-2- 尽管沸点高于乙酸的丁酮不能像其他非乙酸有机杂质那样通过简单蒸馏分离。 本发明的用于除去所述溴 - 酮的技术,其概念是使用低温结晶和去除附着母液的组合,这可以在为其它分级结晶设计的已知装置中连续实施。

    Method for preparing aromatic carboxylic acids
    8.
    发明授权
    Method for preparing aromatic carboxylic acids 失效
    芳香羧酸的制备方法

    公开(公告)号:US5292934A

    公开(公告)日:1994-03-08

    申请号:US900593

    申请日:1992-06-18

    摘要: Disclosed is a method for preparing an aromatic carboxylic acid comprising oxidizing in the liquid phase an aromatic feed compound containing at least one alkyl or acyl group with a molecular oxygen-containing gas, in a solvent comprising a low molecular weight aliphatic carboxylic acid, and in the presence of a heavy metal oxidation catalyst, thereby forming an oxidation reaction product mixture comprising an aromatic carboxylic acid; subsequently heating the oxidation reaction product mixture at a temperature of at least about 500.degree. F. to form a second product mixture; and recovering from the second product mixture the aromatic carboxylic acid. The method of this invention provides for purer, larger particle size aromatic carboxylic acid product.

    摘要翻译: 公开了一种制备芳族羧酸的方法,包括在包含低分子量脂族羧酸的溶剂中在液相中氧化含有至少一个烷基或酰基的含分子氧的气体的芳族进料化合物, 存在重金属氧化催化剂,从而形成包含芳族羧酸的氧化反应产物混合物; 随后在至少约500华氏度的温度下加热氧化反应产物混合物以形成第二产物混合物; 并从第二产物混合物中回收芳族羧酸。 本发明的方法提供了更纯的较大颗粒度的芳族羧酸产物。

    Process for preparing purified aromatic polycarboxylic acids
    10.
    发明授权
    Process for preparing purified aromatic polycarboxylic acids 失效
    制备纯化的芳族多元羧酸的方法

    公开(公告)号:US5770764A

    公开(公告)日:1998-06-23

    申请号:US858362

    申请日:1997-05-19

    CPC分类号: C07C51/487 C07C51/265

    摘要: Economical processes are disclosed for preparing relatively pure polycarboxylic acid from typical crude products of liquid phase oxidation, which do not involve intermediate steps of ester formation or require any alkanol containing solvent, for purification of "crude" polycarboxylic acid containing impurities which include one or more monofunctional aromatic compounds, trifunctional aromatic compounds, and/or color causing organic compounds formed by oxidation of a corresponding substituted aromatic compound in a liquid phase, e.g. 2,6-naphthalene dicarboxylic acid by liquid phase oxidation of 2,6-dimethyl naphthalene. The invention provides integrate processes which comprise reacting crude oxidation product with a polyalkyl amine amine, e.g. trialkylamine, forming an aqueous solution of the salts thus obtained, separating deleterious compounds from the solution, and recovering the polyalkyl amine and a relatively pure polycarboxylic acid product.

    摘要翻译: 公开的经济方法用于从典型的液相氧化粗产物制备相对纯的多元羧酸,其不涉及酯形成的中间步骤或需要任何含链烷醇的溶剂,用于纯化含有一种或多种含杂原子的“粗”多元羧酸 单官能芳族化合物,三官能芳族化合物和/或由液相中相应的取代芳族化合物氧化形成的有色化合物,例如 2,6-萘二甲酸通过液相氧化2,6-二甲基萘。 本发明提供了整合方法,其包括使粗氧化产物与多烷基胺胺反应, 三烷基胺,形成由此获得的盐的水溶液,从溶液中分离有害化合物,并回收多烷基胺和相对纯的多元羧酸产物。