CN112546973B - System and process for producing phthalic acid by enhancing xylene oxidation - Google Patents

System and process for producing phthalic acid by enhancing xylene oxidation Download PDF

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Publication number
CN112546973B
CN112546973B CN201910851918.XA CN201910851918A CN112546973B CN 112546973 B CN112546973 B CN 112546973B CN 201910851918 A CN201910851918 A CN 201910851918A CN 112546973 B CN112546973 B CN 112546973B
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micro
interface generator
bed reactor
slurry bed
liquid
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CN112546973A (en
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张志炳
周政
李磊
张锋
孟为民
王宝荣
杨高东
罗华勋
杨国强
田洪舟
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Nanjing Institute of Microinterface Technology Co Ltd
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Nanjing Institute of Microinterface Technology Co Ltd
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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
    • 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
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • 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
    • 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
    • B01J8/001—Controlling catalytic processes
    • 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
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • 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
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/082—Controlling processes
    • 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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/24—1,3 - Benzenedicarboxylic acid
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/26—1,4 - Benzenedicarboxylic acid
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature

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

Abstract

The invention provides a system and a process for producing phthalic acid by enhancing dimethylbenzene oxidation, which comprises the following steps: a slurry bed reactor, a micro-interface generator, a circulating pipeline, a gas inlet pipeline and a separation unit; wherein the upper part of the slurry bed reactor is communicated with the condensing unit, and the lower part of the slurry bed reactor is communicated with the crystallization filter; the micro-interface generator is arranged in the slurry bed reactor and is used for breaking gas into micro-level micro-bubbles, so that the mass transfer efficiency of gas and liquid is improved, and the reaction pressure is reduced; the circulating pipeline is used for pumping the liquid phase material at the bottom of the slurry bed reactor into the second micro-interface generator; the feed inlet of the separation unit is connected with the condensation unit, and the liquid-phase material outlet of the separation unit is communicated with the liquid-phase material inlet of the first micro-interface generator.

Description

System and process for producing phthalic acid by enhancing xylene oxidation
Technical Field
The invention relates to preparation of phthalic acid, in particular to a system and a process for producing phthalic acid by enhancing oxidation of dimethylbenzene.
Background
Xylene is colorless transparent liquid; is the product of substitution of two hydrogens on the benzene ring by methyl, and there are three isomers of ortho, meta and para, and in industry, xylene refers to the mixture of the above isomers; which can produce phthalic acid, terephthalic acid, isophthalic acid and other substances respectively through oxygen oxidation.
Phthalic acid is colorless crystal or crystalline powder, two carboxyl groups are respectively connected with two adjacent carbon atoms in benzene ring to form binary aromatic carboxyl, and phthalic anhydride can be used for replacing phthalic acid in application. Phthalic acid is a raw material for synthetic resins, fibers, medicines, and the like. Isophthalic acid (IPA for short) is a raw material of polyester resin and is mainly used for preparing polyester bottle chips, fibers, unsaturated resins and low-melting-point polyester products. The production method of IPA is to obtain Crude Isophthalic Acid (CIA) by liquid phase oxidation using meta-xylene (MX) as raw material, and then remove trace impurities in the product by hydrofining to obtain polymer grade IPA. Terephthalic acid is an important commodity chemical produced from para-xylene (PX) by air oxidation.
In the prior art, the reaction pressure in the preparation process method of the phthalic acid is large, so that the danger of a reaction device is increased, and meanwhile, the excessive reaction pressure can cause more energy loss, so that the reaction cost is further increased.
Disclosure of Invention
The present invention provides a system and process for enhanced oxidation of xylenes to produce phthalic acid, which at least partially solves the above-mentioned problems,
in one aspect, the invention provides a system for enhancing the oxidation of xylenes to produce phthalic acid comprising:
the slurry bed reactor is used as a reaction place for oxidizing the dimethylbenzene, acetic acid solvent is filled in the slurry bed reactor, and the upper part of the slurry bed reactor is communicated with the condensing unit and the lower part of the slurry bed reactor is communicated with the crystallization filter;
a first micro-interface generator disposed on a fixed plate within the slurry bed reactor;
a second micro-interface generator disposed inside the slurry bed reactor and below the first micro-interface generator;
the liquid inlet of the circulating pipeline is arranged in the slurry bed reactor and is positioned below the second micro-interface generator, and the liquid outlet of the circulating pipeline is communicated with the liquid phase material inlet of the first micro-interface generator;
the gas inlet pipeline is respectively connected with gas phase material inlets of the first micro-interface generator and the second micro-interface generator;
the feed inlet of the separation unit is connected with the condensation unit, and the liquid-phase material outlet of the separation unit is communicated with the liquid-phase material inlet of the first micro-interface generator.
Further, the solvent in the slurry bed reactor occupies 3/5 to 4/5 of the volume of the slurry bed reactor.
Further, the distance from the fixing plate to the bottom of the slurry bed reactor is more than 2/3 of the total height of the slurry bed reactor.
Further, the heat exchanger is arranged on the circulating pipeline.
Further, the solvent inlet of the slurry bed reactor is located below the first micro-interface generator and above the second micro-interface generator.
Further, the feed conduit of the slurry bed reactor is located below the first micro-interface generator and above the second micro-interface generator.
Further, the catalyst addition conduit of the slurry bed reactor is located below the first micro-interface generator and above the second micro-interface generator.
Further, the first micro-interface generator is a hydraulic micro-interface generator.
Further, the second micro-interface generator is a pneumatic micro-interface generator.
In another aspect, the invention also provides a process for producing phthalic acid by enhanced oxidation of xylenes, comprising;
oxygen enters a first micro-interface generator and a second micro-interface generator through an air inlet pipeline, liquid-phase materials at the bottom of a slurry bed reactor enter the first micro-interface generator through a circulating pipeline, turbulent flow is formed in the first micro-interface generator by the liquid-phase materials, oxygen from the air inlet pipeline is sucked in a entrainment mode, so that a gas-liquid emulsion is formed, the second micro-interface generator breaks the oxygen into micron-level bubbles so as to increase the gas-liquid phase interface area, and the bubbles are dissolved in liquid phase around the second micro-interface generator, so that the gas-liquid emulsion is formed;
meanwhile, after the catalyst enters the slurry bed reactor, under the action of the upward floating thrust of the bubbles discharged by the second micro-interface generator, the catalyst is always suspended in the middle area of the first micro-interface generator and the second micro-interface generator, and the catalyst carries out catalytic reaction on the gas-liquid emulsion in the middle area;
the gas-phase product in the slurry bed reactor sequentially enters a condensing unit and a separating unit, and the liquid-phase product in the separating unit returns to the first micro-interface generator.
Compared with the prior art, the invention has the beneficial effects of improving the mass transfer efficiency of the gas-liquid two phases, reducing the reaction time and reducing the material consumption and energy consumption;
further, a first micro-interface generator and a second micro-interface generator are arranged in the slurry bed reactor, and break up gas into micro-level micro-bubbles, so that the mass transfer efficiency of gas and liquid is improved, and the reaction pressure is reduced;
particularly, the oxygen is broken by the micro-interface generator after entering the reactor, so that the residence time of the gas in the reactor is longer, and the utilization rate of the oxygen is improved;
further, a catalyst adding pipeline is arranged between the first micro-interface generator and the second micro-interface generator, and the catalyst enters the slurry bed reactor and is always suspended in the reactor under the influence of the floating acting force of bubbles broken by the second micro-interface generator below, so that the catalytic efficiency is improved;
further, a circulating pipeline is arranged outside the slurry bed reactor and pumps liquid phase materials at the bottom of the reactor to the first micro-interface generator above the reactor, so that the liquid phase materials in the reactor are always in a flowing state, the condition that reaction products are always accumulated on the surface of the catalyst is avoided, and the temperature control unit also controls the temperature in the reactor by controlling the temperature of the flowing liquid phase materials, thereby ensuring the reaction efficiency.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Detailed Description
In order that the objects and advantages of the invention will become more apparent, the invention will be further described with reference to the following examples; it should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are merely for explaining the technical principles of the present invention, and are not intended to limit the scope of the present invention.
It should be noted that, in the description of the present invention, terms such as "upper," "lower," "left," "right," "inner," "outer," and the like indicate directions or positional relationships based on the directions or positional relationships shown in the drawings, which are merely for convenience of description, and do not indicate or imply that the apparatus or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those skilled in the art according to the specific circumstances.
Referring to FIG. 1, a schematic diagram of a system for producing phthalic acid by enhanced oxidation of xylene according to the present invention is shown, the system comprising: the reactor comprises a slurry bed reactor 1, a first micro-interface generator 2, a solvent inlet 3, a feeding pipeline 4, a catalyst adding pipeline 5, a second micro-interface generator 6, a condensing unit 7, a tail gas discharge port 8, a separating unit 9, a circulating pipeline 10, a gas inlet pipeline 11, a crystallization filter 12 and a solid product outlet 13.
Wherein the gas inlet pipeline 11 is connected with the gas inlet of the first micro-interface generator 2 and the second micro-interface generator 6; the first micro-interface generator 2 is arranged on a fixed plate 21 positioned inside the slurry bed reactor 1, and the micro-interface generator 6 is arranged inside the slurry bed reactor 1 and below the first micro-interface generator 2; a circulation pipe 10 is arranged outside the slurry bed reactor 1 and is used for pumping liquid phase materials at the bottom of the slurry bed into the first micro-interface generator 2 for circulation. The gas phase outlet of the slurry bed reactor 1 is connected with a condensing unit 7, the condensing unit 7 is connected with a separating unit 9, and the liquid phase product outlet of the separating unit 9 is connected with the liquid inlet of the slurry bed reactor 1; the liquid phase outlet of the slurry bed reactor 1 is connected to a crystallization filter 12 and the filtered crystalline material is discharged through a solid product outlet 13. It will be appreciated by those skilled in the art that in the system of the present invention, the pipes connecting the above devices may be provided with valves or pumps, etc. for controlling the flow of the liquid phase material in the pipes.
The invention also provides a process method for producing phthalic acid by enhancing the oxidation of dimethylbenzene, which comprises the following steps:
oxygen enters a first micro-interface generator and a second micro-interface generator through an air inlet pipeline, liquid-phase materials at the bottom of a slurry bed reactor enter the first micro-interface generator through a circulating pipeline, turbulent flow is formed in the first micro-interface generator by the liquid-phase materials, oxygen from the air inlet pipeline is sucked in a entrainment mode, so that a gas-liquid emulsion is formed, the second micro-interface generator breaks the oxygen into micron-level bubbles so as to increase the gas-liquid phase interface area, and the bubbles are dissolved in liquid phase around the second micro-interface generator, so that the gas-liquid emulsion is formed;
meanwhile, after the catalyst enters the slurry bed reactor, under the action of the upward floating thrust of the bubbles discharged by the second micro-interface generator, the catalyst is always suspended in the middle area of the first micro-interface generator and the second micro-interface generator, and the catalyst carries out catalytic reaction on the gas-liquid emulsion in the middle area;
the gas-phase product in the slurry bed reactor sequentially enters a condensing unit and a separating unit, and the liquid-phase product in the separating unit returns to the first micro-interface generator.
It will be appreciated by those skilled in the art that the type of catalyst used in the present process is not limited in any way, as long as the reaction conditions are satisfied.
Example 1
Oxidizing o-xylene with the purity of 98% to prepare phthalic acid, when the reaction is started, firstly closing a valve 14 and a valve 15, enabling an acetic acid solvent and the o-xylene to enter a slurry bed reactor to form a mixed solution, enabling oxygen to enter a second micro-interface generator to be smashed into micron-sized bubbles, and forming a gas-liquid emulsion with the surrounding mixed solution; meanwhile, the catalyst enters the slurry bed reactor from a catalyst adding pipeline above the second micro-interface generator and is suspended in the slurry bed reactor under the action of upward floating of micron-sized bubbles broken by the second micro-interface generator; after 47 minutes, the valve 14 and the valve 15 are opened, the temperature control circulation unit starts to work, liquid phase materials at the bottom of the slurry bed reactor are pumped out, cooled by the heat exchanger, and then are fed into the liquid phase inlet of the first micro-interface generator together with the liquid phase materials separated by the separation unit, meanwhile, oxygen enters the gas phase inlet of the first micro-interface generator, the liquid phase materials form turbulence in the first micro-interface generator, and the entered oxygen is sucked up to form gas-liquid emulsion, so that the reaction rate is accelerated, and the reaction pressure is reduced.
The technical effects of this embodiment are: the reaction pressure is not more than 2MPa all the time, the reaction temperature is kept at 120-150 ℃ under the condition of keeping the pressure at 1.5-2MPa, the conversion rate of o-xylene is 97%, and the yield of phthalic acid is 95%.
Example 2
The m-xylene with the purity of 99.5 percent is used as a raw material to prepare the isophthalic acid by oxidation, the reaction pressure is 1.5MPa, and the weight ratio of the solvent to the m-xylene in the slurry bed reactor is 4:1, when the reaction starts, the valve 14 and the valve 15 are in a closed state, acetic acid solvent and m-xylene enter a slurry bed reactor to form a mixed solution, oxygen enters a second micro-interface generator to be smashed into micron-sized bubbles, and a gas-liquid emulsion is formed with the surrounding mixed solution; meanwhile, the catalyst enters the slurry bed reactor from a catalyst adding pipeline above the second micro-interface generator and is suspended in the slurry bed reactor under the action of upward floating of micron-sized bubbles broken by the second micro-interface generator; after 47 minutes, the valve 14 and the valve 15 are opened, the temperature control circulation unit starts to work, liquid phase materials at the bottom of the slurry bed reactor are pumped out, cooled by the heat exchanger, and then are fed into the liquid phase inlet of the first micro-interface generator together with the liquid phase materials separated by the separation unit, meanwhile, oxygen enters the gas phase inlet of the first micro-interface generator, the liquid phase materials form turbulence in the first micro-interface generator, and the entered oxygen is sucked up to form gas-liquid emulsion, so that the reaction rate is accelerated, and the reaction pressure is reduced.
The technical effects of this embodiment are: the reaction pressure is not more than 1.8MPa all the time, the reaction temperature is kept at 150-170 ℃ under the condition of keeping the pressure at 1.5-1.8MPa, the conversion rate of m-xylene is 98%, and the yield of isophthalic acid is 95%.
Example 3
The p-xylene is used as a raw material to prepare terephthalic acid by oxidation, the reaction pressure is 1.45MPa, and the mass ratio of the p-xylene to the acetic acid solvent to the catalyst is (1): 3:0.001; when the reaction is started, the acetic acid solvent and the paraxylene enter a slurry bed reactor to form a mixed solution, and oxygen enters a second micro-interface generator to be smashed into micron-sized bubbles, so that a gas-liquid emulsion is formed with the surrounding mixed solution; meanwhile, the catalyst enters the slurry bed reactor from a catalyst adding pipeline above the second micro-interface generator and is suspended in the slurry bed reactor under the action of upward floating of micron-sized bubbles broken by the second micro-interface generator; the temperature control circulating unit extracts liquid phase materials at the bottom of the slurry bed reactor, the liquid phase materials are heated or cooled to 150 ℃ through the heat exchanger and then are sent into the liquid phase inlet of the first micro-interface generator together with the liquid phase materials separated by the separating unit, meanwhile, oxygen enters the gas phase inlet of the first micro-interface generator, the liquid phase materials form turbulence in the first micro-interface generator, the entered oxygen is sucked up, and a gas-liquid emulsion is formed, so that the reaction rate is accelerated, and the reaction pressure is reduced.
The technical effects of this embodiment are: the conversion rate of the paraxylene is 97% -99%, and the yield of the terephthalic acid is 98%.

Claims (8)

1. A system for enhancing the oxidation of xylenes to produce phthalic acid, comprising:
the slurry bed reactor is used as a reaction place for oxidizing the dimethylbenzene, acetic acid solvent is filled in the slurry bed reactor, and the upper part of the slurry bed reactor is communicated with the condensing unit and the lower part of the slurry bed reactor is communicated with the crystallization filter;
the first micro-interface generator is a hydraulic micro-interface generator and is arranged on a fixed plate in the slurry bed reactor;
the second micro-interface generator is selected as a pneumatic micro-interface generator, is arranged inside the slurry bed reactor and is positioned below the first micro-interface generator;
the liquid inlet of the circulating pipeline is arranged in the slurry bed reactor and is positioned below the second micro-interface generator, and the liquid outlet of the circulating pipeline is communicated with the liquid phase material inlet of the first micro-interface generator;
the gas inlet pipeline is respectively connected with gas phase material inlets of the first micro-interface generator and the second micro-interface generator; the feed inlet of the separation unit is connected with the condensation unit, and the liquid-phase material outlet of the separation unit is communicated with the liquid-phase material inlet of the first micro-interface generator.
2. The system for enhanced oxidation of xylenes to produce phthalic acid of claim 1, wherein the solvent in the slurry bed reactor is 3/5 to 4/5 of the volume of the slurry bed reactor.
3. The system for enhanced oxidation of xylenes to produce phthalic acid of claim 1, wherein the distance of the fixed plate from the bottom of the slurry bed reactor is greater than 2/3 of the total height of the slurry bed reactor.
4. The system for enhanced oxidation of xylenes to produce phthalic acid of claim 1, further comprising a heat exchanger disposed on the recycle line.
5. The enhanced xylene oxidation to produce phthalic acid system according to claim 1, wherein the solvent inlet of the slurry bed reactor is located below the first micro-interface generator and above the second micro-interface generator.
6. The enhanced xylene oxidation to produce phthalic acid system according to claim 1, wherein the feed conduit of the slurry bed reactor is located below the first micro-interface generator and above the second micro-interface generator.
7. The enhanced xylene oxidation to produce phthalic acid system according to claim 1, wherein the catalyst addition conduit of the slurry bed reactor is located below the first micro-interface generator and above the second micro-interface generator.
8. A process for enhancing a system for producing phthalic acid by oxidation of xylene as claimed in any of claims 1 to 7, comprising;
oxygen enters a first micro-interface generator and a second micro-interface generator through an air inlet pipeline, liquid-phase materials at the bottom of a slurry bed reactor enter the first micro-interface generator through a circulating pipeline, turbulent flow is formed in the first micro-interface generator by the liquid-phase materials, oxygen from the air inlet pipeline is sucked in a entrainment mode, so that a gas-liquid emulsion is formed, the second micro-interface generator breaks the oxygen into micron-level bubbles so as to increase the gas-liquid phase interface area, and the bubbles are dissolved in liquid phase around the second micro-interface generator, so that the gas-liquid emulsion is formed;
meanwhile, after the catalyst enters the slurry bed reactor, under the action of the upward floating thrust of the bubbles discharged by the second micro-interface generator, the catalyst is always suspended in the middle area of the first micro-interface generator and the second micro-interface generator, and the catalyst carries out catalytic reaction on the gas-liquid emulsion in the middle area; the gas-phase product in the slurry bed reactor sequentially enters a condensing unit and a separating unit, and the liquid-phase product in the separating unit returns to the first micro-interface generator.
CN201910851918.XA 2019-09-10 2019-09-10 System and process for producing phthalic acid by enhancing xylene oxidation Active CN112546973B (en)

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CN113512483A (en) * 2021-07-14 2021-10-19 南京延长反应技术研究院有限公司 Device and method for enhancing biological fermentation of ultra-efficient low-pressure gas source micro-interface
CN113546583A (en) * 2021-07-16 2021-10-26 南京延长反应技术研究院有限公司 Micro-interface preparation system and preparation method of DMC

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