WO2010081358A1 - 生产对苯二甲酸的px氧化反应器 - Google Patents

生产对苯二甲酸的px氧化反应器 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
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Prior art keywords
reactor
terephthalic acid
producing terephthalic
oxidation reactor
air
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PCT/CN2009/075384
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English (en)
French (fr)
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
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China National Petroleum Corp
China Textile Industrial Engineering Institute
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China National Petroleum Corp
China Textile Industrial Engineering Institute
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Priority to RU2011133892/04A priority Critical patent/RU2505524C2/ru
Publication of WO2010081358A1 publication Critical patent/WO2010081358A1/zh
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    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

说 明 书
生产对苯二曱酸的 PX氧化反应器 技术领域
本发明涉及化工设备领域， 尤其涉及一种生产对苯二曱酸的 PX 氧化反应器。
背景技术
精对苯二曱酸（PTA ) 工艺生产过程是： 原料对二曱苯（PX )和 溶剂醋酸（HAC ) 的混合物， 在催化剂存在的条件下， 与空气中的氧 气在一定的温度和压力下进行氧化反应， 生成粗对苯二曱酸（CTA ), 并进一步对 CTA进行精制处理， 最终生成精对苯二曱酸（PTA )。
PX 氧化反应器是此工艺流程中的关键设备， 不同的工艺流程氧 化反应器有不同的结构形式。从强化传质过程考虑反应器结构形式可 分为两种类型： 第一类是无搅拌鼓泡塔式反应器； 第二类是带搅拌器 的釜式反应器， 这两类结构形式的氧化反应器， 都可以进行生产， 所 不同的是， 装备的一次投入和长年能耗等方面存在较大差别； 按反应 条件可分为三种情况： 高温氧化工艺 （191 ~ 205 °C )、 中温氧化工艺 ( 185 ~ 189 °C )和低温氧化工艺 ( 160 ~ 170 °C )。
当前国际上 PTA生产主要釆用高温氧化工艺，高温氧化工艺反应 速率快， 釆用搅拌釜强化传质与传热， 单位容积生产能力高， CTA晶 体粒径较大， 反应浆料中允许含水量高， 不足的是 PX和 HAC消耗较 高， 搅拌器及压缩机造价高， 装备制造难度大； 比中温氧化工艺对设 备的要求及 PX和 HAC消耗均比较适中， 反应器可以釆用结构简单的 鼓泡塔来代替搅拌釜， 设备投入及维修费用低， 能耗低， CTA的分离 与母液处理又比低温过程容易得多，该工艺的各项技术经济指标也类 同或略好于高温氧化工艺；而低温氧化工艺釆用无搅拌鼓泡塔即可满 足传质要求， PX和 HAC消耗低， 不足之处是要求反应浆料中含水量 低， 同时杂质含量高、浆料必需进行后氧化， 晶体粒径小， 残渣量大， 仅适合于制备中纯度对苯二曱酸（MTA或 QTA ) 而不适合生产 PTA。 发明内容
本发明的目的在于克服现有技术的缺陷，提供一种生产对苯二曱 酸的新型 PX氧化反应器， 以达到节省能量， 减少投资、 降低成本、 工艺简单， 实现大型化生产对苯二曱酸的目的。
本发明是通过以下技术方案实现的：
一种生产对苯二曱酸的 PX氧化反应器， 包括反应器壳体， 所述 反应器壳体通常呈塔形， 其高径比优选 2. 8 ~ 5 , 所述反应器壳体底 部设有分布式进气装置和旋流式进气装置。
所述分布式进气装置可以包括若干气流分布管，所述气流分布管 通常可以呈圓环形， 其圓心在所述壳体的垂直中线上， 管体上设有若 干个通气孔。
所述气流分布管通常可以包括外环气流分布管和内环气流分布 管， 所述外环气流分布管接近所述壳体的内壁， 所述内环气流分布管 位于壳体内空间的中部 （指水平方向上， 下同）， 所述外环气流分布 管和内环气流分布管连接有进气管。
所述旋流进气装置可以由若干旋流进气管构成，位于上述气流分 布管的下方。 当所述旋流进气管的数量是多个时， 一般应均匀分布在 所述壳体内壁的四周。
本发明釆用了由分布式进气装置和旋流式进气装置构成的组合 式进气装置， 以适当量的空气推动反应器底部流体， 使之发生旋转运 动， 气体分散良好， 分布均匀， 减少偏流， 可满足固体悬浮的需要， 所釆用的旋流式气体分布管可以有效的消除底部流动死区，保持物料 能处于正常的悬浮状态，从而保证反应器的长年安全稳定运行； 并且 壳体釆用介于高温与低温反应器之间的高径比，相应的空塔气速也介 于二者之间， 即能保证良好的气液传质与混合， 又能满足固体均匀悬 浮要求， 塔物料混合良好， 温度与浓度分布均匀， 既避免了高径比大 的低温反应器内存在的不均匀分布的现象，又以低动力消耗优于高温 反应器；所用的分布式进气装置釆用环形的外环和内环两个气流分布 管结构， 同旋流进气管形成的旋流相配合， 可以保证有效地的进气量 以及空气分布和传质， 不仅结构简单， 而且避免了对旋流的破坏， 不 产生死角， 避免反应产生的晶体的沉积。
附图说明
图 1是本发明所述的生产对苯二曱酸的 PX氧化反应器的主视图； 图 2是本发明所述的生产对苯二曱酸的 PX氧化反应器的底部横 断面的俯视图。
具体实施方式
参见图 1-2 , 本发明所述的生产对苯二曱酸的 PX氧化反应器， 包括反应器壳体 1 , 所述反应器壳体 1底部设有分布式进气装置和旋 流式进气装置。 所述反应器壳体 1一般可以呈塔形， 其高径比优选为 2. 8 ~ 5 , 这种高径比的空塔气速介于高温与低温反应器之间，既避免了高径比 大的低温反应器内存在的不均匀分布的现象，又以低动力消耗优于高 温反应器。
所述分布式进气装置可以包括若干气流分布管 2 (例如图 2中所 示的外环气流分布管 4和内环气流分布管 5 ), 所述气流分布管 2呈 圓环形， 其圓心在所述壳体的垂直中线上， 管体上设有若干个通气孔 7 , 这种进气装置在保证供气布气的同时， 与其下方的旋流进气管 3 构成的旋流进气装置相配合， 可以明显地提高气体的分散效果，保证 空气分布均匀， 保持物料能处于正常的悬浮状态， 可以避免对旋流的 破坏， 避免出现死角。
所述气流分布管一般可以包括外环气流分布管 4 和内环气流分 布管 5 , 所述外环气流分布管 4接近壳体内壁， 所述内环气流分布管 5位于壳体中部， 所喷出的气流可防止反应器边壁效应过大时出现的 环形返流；所述外环气流分布管 4和内环气流分布管 5连接进气管 6 , 内环分布管 5位于器体中部， 主要起强化反应器中部的传质作用。
所述内环气流分布管 5的高度（垂直位置）可以与所述外环气流 分布管 4相同， 也可以比所述外环气流分布管 4低， 以改善壳体下部 中央部位的供气状况。
所述气流分布管 2通常可以连接有支撑件 8。
所述旋流进气装置可以由若干旋流进气管 3构成，通常位于所述 气流分布管 2的下方。 当所述旋流进气管 3的数量是多个时， 一般应 均匀分布在所述壳体内壁的四周。这种所述旋流进气装置可以形成良 好的旋流， 并且在驱使液流旋动的同时， 也提供反应所需的部分空气 量。
所述旋流进气管 3的出气段相对于罐体半径可倾斜 45 ~ 60。 , 以便形成适当的旋流。 在相同流量下， 通常可以控制位于下部的内环 旋流进气管的流量为位于上部的外环气流分布管的流量的 0. 3 ~ 0. 5 倍时， 这样可以获得优良的气泡分散效果， 同时提高整体气含率。
所述反应器壳体 1上部为气液分离段， 设有填料层 9 , 所述填料 层 9填充有规整填料 10 , 能够同时脱水、 除沫和回收固体， 填料层 9 的上部通常可安装有回流分布器， 上下方留有分离空间， 以利于分离 上升气流夹带的 TA固体和醋酸溶剂等。 所述气液分离段的中上部可 设有回流口 11 , 顶部可设有气相出口 12。
所述反应器壳体 1底部为鼓泡区，所述反应器壳体底部封头优选 球形封头 ,封头的容积内通过多个均勾分布的旋流进气管多部位立体 进气， 使气液接触既充分均匀， 不留死区， 液体有规律的旋转运动， 使器壁自清洗， 所述封头底部开有出料口 1 3。 釆用球形封头可以避 免碟形、椭圓形等其他形状封头存在的小直径过渡段，有利于反应生 成物顺利地由出料口 1 3排出。
所述反应器壳体 1 中部为非均相反应段， 其中下部设有进料口 14 , 反应物料和催化剂充分混合后从进料口 14加入反应器， 与从底 部上升的空气充分接触 ， 完成氧化反应。

Claims

权 利 要 求 书
1、 一种生产对苯二曱酸的 PX氧化反应器， 其特征在于： 包括反 应器壳体，所述反应器壳体底部设有分布式进气装置和旋流式进气装 置。
2、如权利要求 1所述的生产对苯二曱酸的 PX氧化反应器， 其特 征在于： 所述分布式进气装置包括若干气流分布管， 所述气流分布管 呈圓环形， 其圓心在所述壳体的垂直中线上， 所述气流分布管上设有 若干个通气孔。
3、如权利要求 2所述的生产对苯二曱酸的 PX氧化反应器， 其特 征在于： 所述气流分布管包括外环气流分布管和内环气流分布管， 所 述外环气流分布管接近所述壳体的内壁，所述内环气流分布管位于壳 体内的中部， 所述外环气流分布管和内环气流分布管均连接有进气 管。
4、 如权利要求 1、 2或 3 所述的生产对苯二曱酸的 PX氧化反应 器， 其特征在于： 所述旋流进气装置由若干旋流进气管构成， 位于所 述气流分布管的下方。
5、如权利要求 4所述的生产对苯二曱酸的 PX氧化反应器， 其特 征在于： 所述旋流进气管的数量是多个， 均勾分布在所述壳体内壁的 四周。
6、如权利要求 5所述的生产对苯二曱酸的 PX氧化反应器， 其特 征在于： 所述气流分布管连接有支撑件，旋流进气管的出气段相对于 罐体半径倾斜 45 ~ 60。 。
7、如权利要求 6所述的生产对苯二曱酸的 PX氧化反应器， 其特 征在于： 所述反应器壳体上部设有填料层， 所述填料层填充有规整填 料， 填料层的上部安装有回流分布器， 上下方留有分离空间。
8、 如权利要求 7所述的生产对苯二曱酸的 PX氧化反应器， 其 特征在于： 所述反应器壳体底部设有球形封头， 所述球形封头的底部 开有出料口。
9、如权利要求 8所述的生产对苯二曱酸的 PX氧化反应器， 其特 征在于： 所述反应器壳体中下部设有进料口， 上部设有回流口， 顶部 可设有气相出口。
10、 如权利要求 9所述的生产对苯二曱酸的 PX氧化反应器， 其 特征在于： 所述反应器壳体呈塔形， 其高径比为 2. 8 ~ 5。
PCT/CN2009/075384 2009-01-15 2009-12-08 生产对苯二甲酸的px氧化反应器 Ceased WO2010081358A1 (zh)

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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
CN115849548A (zh) * 2022-12-01 2023-03-28 南京环保产业创新中心有限公司 一种臭氧氧化反应装置

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