WO2010081358A1 - Réacteur d'oxydation du paraxylène destiné à produire de l'acide téréphtalique - Google Patents

Réacteur d'oxydation du paraxylène destiné à produire de l'acide téréphtalique Download PDF

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Publication number
WO2010081358A1
WO2010081358A1 PCT/CN2009/075384 CN2009075384W WO2010081358A1 WO 2010081358 A1 WO2010081358 A1 WO 2010081358A1 CN 2009075384 W CN2009075384 W CN 2009075384W WO 2010081358 A1 WO2010081358 A1 WO 2010081358A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
terephthalic acid
producing terephthalic
oxidation reactor
air
Prior art date
Application number
PCT/CN2009/075384
Other languages
English (en)
Chinese (zh)
Inventor
罗文德
周华堂
姚瑞奎
张莼
李利军
汪英枝
谢祥志
张亚丹
劳国瑞
郑皓
陈襄颐
Original Assignee
中国石油天然气集团公司
中国纺织工业设计院
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 中国石油天然气集团公司, 中国纺织工业设计院 filed Critical 中国石油天然气集团公司
Priority to RU2011133892/04A priority Critical patent/RU2505524C2/ru
Publication of WO2010081358A1 publication Critical patent/WO2010081358A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
    • C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
    • C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
    • C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups

Definitions

  • the invention relates to the field of chemical equipment, and in particular to a PX oxidation reactor for producing terephthalic acid.
  • the production process of the purified terephthalic acid (PTA) process is: a mixture of the raw material p-benzoquinone (PX) and the solvent acetic acid (HAC), in the presence of a catalyst, with oxygen in the air at a certain temperature and pressure.
  • the oxidation reaction is carried out to form crude terephthalic acid (CTA), and the CTA is further refined to finally produce purified terephthalic acid (PTA).
  • PX oxidation reactors are key equipment in this process, and different process oxidation reactors have different structural forms.
  • the first type is a stirred bubble column reactor; the second type is a tank reactor with a stirrer, and the oxidation of these two types of structures
  • the reactor can be produced.
  • the difference is that there is a big difference between the equipment's primary input and long-term energy consumption.
  • the reaction conditions it can be divided into three cases: high temperature oxidation process (191 ⁇ 205 °C), Medium temperature oxidation process (185 ⁇ 189 °C) and low temperature oxidation process (160 ⁇ 170 °C).
  • PTA production in the world mainly uses high-temperature oxidation process, high-temperature oxidation process has a fast reaction rate, and uses a stirred tank to enhance mass transfer and heat transfer, high productivity per unit volume, large particle size of CTA crystal, and allowable water content in the reaction slurry.
  • High the shortage is high PX and HAC, the cost of the agitator and compressor is high, and the equipment manufacturing is difficult; the requirements of the medium temperature oxidation process and the PX and HAC consumption are relatively moderate, and the reactor can be simple in structure.
  • Bubbling tower instead of stirred tank, low equipment input and maintenance costs, low energy consumption, separation of CTA It is much easier to process with mother liquor than the low temperature process.
  • the object of the present invention is to overcome the defects of the prior art and provide a novel PX oxidation reactor for producing terephthalic acid to save energy, reduce investment, reduce cost, and simple process, and realize large-scale production of parabens.
  • the purpose of the acid is to overcome the defects of the prior art and provide a novel PX oxidation reactor for producing terephthalic acid to save energy, reduce investment, reduce cost, and simple process, and realize large-scale production of parabens.
  • the reactor housing is provided with a columnar shape, preferably having a height-to-diameter ratio of 2. 8 ⁇ 5 , and the bottom of the reactor housing is provided. There are distributed air intake devices and swirling air intake devices.
  • the distributed air intake device may include a plurality of air flow distribution tubes, and the air flow distribution tubes may generally have a circular shape with a center on a vertical center line of the casing, and a plurality of vent holes are provided in the pipe body.
  • the air distribution tube may generally include an outer ring air distribution tube and an inner ring air distribution tube, the outer ring air distribution tube is adjacent to an inner wall of the housing, and the inner ring air distribution tube is located at a middle portion of the inner space of the housing. In the horizontal direction, the same below), the outer ring air distribution pipe and the inner ring air distribution pipe are connected with an intake pipe.
  • the swirling air intake device may be constituted by a plurality of swirling air intake tubes located below the air flow distributing tubes.
  • the number of the swirling intake pipes is plural, it should generally be evenly distributed The periphery of the inner wall of the housing.
  • the invention adopts a combined air intake device composed of a distributed air intake device and a swirling air intake device, and pushes the fluid at the bottom of the reactor with an appropriate amount of air to make a rotary motion, and the gas is well dispersed and evenly distributed. Reduce the drift, can meet the needs of solid suspension, the use of the swirling gas distribution tube can effectively eliminate the bottom flow dead zone, keep the material in a normal suspension state, thus ensuring the safe and stable operation of the reactor for many years;
  • the shell has a high aspect ratio between the high temperature and low temperature reactors, and the corresponding superficial gas velocity is also between the two, which can ensure good gas-liquid mass transfer and mixing, and can satisfy the uniform suspension of solids.
  • the device adopts two annular flow distribution tube structures of the outer ring and the inner ring, which cooperate with the swirl flow formed by the swirling intake pipe to ensure effective advancement. And air amount and the distribution of mass transfer, not only simple in structure, and avoid damage to the swirling flow, no dead space, avoiding deposition of crystals produced by the reaction.
  • Fig. 1 is a front view showing a PX oxidation reactor for producing terephthalic acid according to the present invention
  • Fig. 2 is a plan view showing a bottom cross section of a PX oxidation reactor for producing terephthalic acid according to the present invention.
  • a PX oxidation reactor for producing terephthalic acid includes a reactor casing 1 , and a distributed air intake device and a swirling inlet are arranged at the bottom of the reactor casing 1 .
  • the reactor housing 1 can be generally in the shape of a tower, and has a height-to-diameter ratio of preferably 2. 8 ⁇ 5 .
  • the high-diameter ratio of the superficial gas velocity is between the high-temperature and low-temperature reactors, thereby avoiding the high diameter.
  • the uneven distribution phenomenon existing in the large-scale low-temperature reactor is superior to the high-temperature reactor with low power consumption.
  • the distributed air intake device may include a plurality of air distribution tubes 2 (such as the outer ring air distribution tube 4 and the inner ring air distribution tube 5 shown in FIG. 2), the air distribution tube 2 is in a circular shape, and its center is at The vertical center line of the casing is provided with a plurality of vent holes 7 on the pipe body.
  • the air intake device is provided with a swirling air intake device formed by the swirling air intake pipe 3 below the gas supply and air supply. Coordination can significantly improve the dispersion effect of the gas, ensure uniform air distribution, keep the material in a normal suspension state, avoid damage to the swirl, and avoid dead spots.
  • the air distribution tube can generally include an outer ring air distribution tube 4 and an inner ring air distribution tube 5, the outer ring air distribution tube 4 is adjacent to the inner wall of the housing, and the inner ring air distribution tube 5 is located at the middle of the housing.
  • the air flow can prevent the annular backflow that occurs when the side wall effect of the reactor is too large; the outer ring air distribution pipe 4 and the inner ring air distribution pipe 5 are connected to the intake pipe 6, and the inner ring distribution pipe 5 is located in the middle of the body, mainly It enhances the mass transfer in the middle of the reactor.
  • the height (vertical position) of the inner ring air distribution tube 5 may be the same as the outer ring air distribution tube 4, or may be lower than the outer ring air distribution tube 4 to improve the air supply status at the central portion of the lower portion of the housing. .
  • the gas distribution tube 2 can usually be connected to a support member 8.
  • the swirling air intake device may be constituted by a plurality of swirling air intake pipes 3, usually below the air flow distributing pipe 2.
  • the number of the swirling intake pipes 3 is plural, generally It is evenly distributed around the inner wall of the casing.
  • Such a swirling air intake device can form a good swirling flow and, while driving the swirling of the liquid stream, also provides a portion of the amount of air required for the reaction.
  • the outlet section of the swirling intake pipe 3 can be inclined by 45 to 60 with respect to the radius of the can body. , in order to form a proper swirl.
  • the overall gas holdup rate is increased.
  • the upper part of the reactor casing 1 is a gas-liquid separation section, and a packing layer 9 is provided.
  • the packing layer 9 is filled with a structured packing 10, which can simultaneously dehydrate, defoam and recover solids.
  • the upper part of the packing layer 9 can usually be installed.
  • the reflux distributor has a separation space above and below to facilitate separation of TA solids and acetic acid solvent entrained in the ascending air stream.
  • the middle portion of the gas-liquid separation section may be provided with a return port 11 and the top portion may be provided with a vapor phase outlet 12.
  • the bottom of the reactor housing 1 is a bubbling zone, and the bottom of the reactor housing is preferably a spherical head, and the volume of the head is multi-dimensionally intakeed through a plurality of swirling intake manifolds of the respective hooks.
  • the gas-liquid contact is sufficiently uniform, leaving no dead zone, and the liquid has a regular rotating motion, so that the wall is self-cleaning, and the discharge port 13 is opened at the bottom of the head.
  • the spherical head can avoid the small diameter transition section of other shape heads such as a dish or an ellipse, which is favorable for the reaction product to be smoothly discharged from the discharge port 13.
  • the middle part of the reactor casing 1 is a heterogeneous reaction section, wherein the lower part is provided with a feed port 14, and the reaction material and the catalyst are thoroughly mixed and then fed into the reactor from the feed port 14 to be in full contact with the air rising from the bottom. Oxidation reaction.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne un réacteur d'oxydation du paraxylène destiné à produire de l'acide téréphtalique qui comprend une coque de réacteur (1). La coque de réacteur (1) est sous forme de tour et a un rapport d'aspect de 2,8 ~ 5. Un dispositif dispersé de prise d'air et un dispositif cyclonique de prise d'air sont disposés dans le fond de la coque du réacteur (1). Le dispositif dispersé de prise d'air comprend un tube (4) de distribution d'air dans l'anneau externe et un tube (5) de distribution d'air dans l'anneau interne, les tubes (2) de distribution d'air étant de forme circulaire. Le dispositif cyclonique de prise d'air comprend de multiples tubes (3) de prise d'air cyclonique lesquels sont distribués uniformément autour de la paroi de la cuve. En adoptant un dispositif tournant combiné de prise d'air, on peut forcer le fluide au fond du réacteur à tourner grâce à une quantité adéquate d'air, et le réacteur présente une bonne dispersion de l'air, maintenant ainsi les matières dans un état de suspension normal. De plus, en adoptant un rapport d'aspect entre celui du réacteur à température élevée et celui du réacteur à faible température, on peut à la fois éviter un phénomène de mauvaise distribution se produisant dans le réacteur à faible température et avoir une plus faible consommation d'énergie, meilleure que celle du réacteur à température élevée.
PCT/CN2009/075384 2009-01-15 2009-12-08 Réacteur d'oxydation du paraxylène destiné à produire de l'acide téréphtalique WO2010081358A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
RU2011133892/04A RU2505524C2 (ru) 2009-01-15 2009-12-08 Реактор окисления параксилола для получения терефталевой кислоты

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN200910076703.1 2009-01-15
CN200910076703A CN100594972C (zh) 2009-01-15 2009-01-15 生产对苯二甲酸的px氧化反应器

Publications (1)

Publication Number Publication Date
WO2010081358A1 true WO2010081358A1 (fr) 2010-07-22

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CN (1) CN100594972C (fr)
RU (1) RU2505524C2 (fr)
WO (1) WO2010081358A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100594972C (zh) * 2009-01-15 2010-03-24 中国纺织工业设计院 生产对苯二甲酸的px氧化反应器
CN101817744B (zh) * 2010-04-30 2013-07-10 中国石油天然气集团公司 对二甲苯氧化结晶装置
CN110013814A (zh) * 2019-04-15 2019-07-16 嘉兴石化有限公司 一种大容量氧化反应器进气系统及其使用方法
CN111389314B (zh) * 2020-03-31 2020-12-11 南京延长反应技术研究院有限公司 Px生产pta的内置微界面机组强化反应系统及工艺
CN111569799B (zh) * 2020-03-31 2023-03-10 南京延长反应技术研究院有限公司 Px生产pta的外置微界面机组强化反应系统及工艺
CN113694837A (zh) * 2020-05-21 2021-11-26 中国石油化工股份有限公司 一种用于不饱和聚合物加氢的釜式反应器和方法及一种丁腈橡胶加氢的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3660476A (en) * 1968-10-30 1972-05-02 Teijin Ltd Method for the preparation of terephthalic acid
CN1634848A (zh) * 2004-10-19 2005-07-06 浙江大学 对苯二甲酸的生产方法与装置
US20060047159A1 (en) * 2004-09-02 2006-03-02 Wonders Alan G Optimized liquid-phase oxidation
CN1806906A (zh) * 2005-01-18 2006-07-26 中国石化上海石油化工股份有限公司 气流搅拌的制备对苯二甲酸的氧化反应装置
CN101513601A (zh) * 2009-01-15 2009-08-26 中国纺织工业设计院 生产对苯二甲酸的px氧化反应器

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2363534C2 (ru) * 2004-09-02 2009-08-10 Истман Кемикал Компани Оптимизированное жидкофазное окисление в барботажной колонне реакторного типа

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3660476A (en) * 1968-10-30 1972-05-02 Teijin Ltd Method for the preparation of terephthalic acid
US20060047159A1 (en) * 2004-09-02 2006-03-02 Wonders Alan G Optimized liquid-phase oxidation
CN1634848A (zh) * 2004-10-19 2005-07-06 浙江大学 对苯二甲酸的生产方法与装置
CN1806906A (zh) * 2005-01-18 2006-07-26 中国石化上海石油化工股份有限公司 气流搅拌的制备对苯二甲酸的氧化反应装置
CN101513601A (zh) * 2009-01-15 2009-08-26 中国纺织工业设计院 生产对苯二甲酸的px氧化反应器

Also Published As

Publication number Publication date
RU2011133892A (ru) 2013-02-20
CN101513601A (zh) 2009-08-26
CN100594972C (zh) 2010-03-24
RU2505524C2 (ru) 2014-01-27

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