CN213078425U - Control system for producing terephthalic acid by oxidizing m-xylene - Google Patents
Control system for producing terephthalic acid by oxidizing m-xylene Download PDFInfo
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- CN213078425U CN213078425U CN201921498349.7U CN201921498349U CN213078425U CN 213078425 U CN213078425 U CN 213078425U CN 201921498349 U CN201921498349 U CN 201921498349U CN 213078425 U CN213078425 U CN 213078425U
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- interface generator
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 title claims abstract description 46
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 230000001590 oxidative effect Effects 0.000 title claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 72
- 239000000463 material Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000007791 liquid phase Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000005086 pumping Methods 0.000 claims abstract description 18
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 239000012071 phase Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims abstract description 4
- 230000005494 condensation Effects 0.000 claims abstract description 4
- 230000000694 effects Effects 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 19
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- 230000003647 oxidation Effects 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000000839 emulsion Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 238000005191 phase separation Methods 0.000 claims description 2
- 238000004148 unit process Methods 0.000 claims description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
An intelligent control system for producing terephthalic acid by oxidizing meta-xylene, comprising: the system comprises a slurry bed reactor, a first micro-interface generator, a second micro-interface generator, a condensation unit, a separation unit, a temperature control circulation unit and a crystallization filter; the slurry bed reactor is used as a reaction place for oxidizing the dimethylbenzene, and liquid-phase phthalic acid is filled in the slurry bed reactor; at least one first micro-interface generator is arranged on a fixed plate positioned in the slurry bed reactor; at least one second micro-interface generator is arranged in the slurry bed reactor and is positioned below the first micro-interface generator; the system of the utility model is also provided with a temperature control circulating unit which is used for pumping the liquid at the bottom of the slurry bed reactor to the liquid phase inlet of the second micro-interface generator so as to achieve the effect of circulating the solvent in the reactor; the utility model discloses a set up devices such as micro-interface generator in the reactor and improved the double-phase mass transfer efficiency of gas-liquid, reduced reaction time, reduced the material consumption energy consumption.
Description
Technical Field
The utility model relates to a preparation of terephthalic acid, concretely relates to system for producing terephthalic acid by oxidizing m-xylene.
Background
Xylene is a colorless transparent liquid; is a product of which two hydrogens on a benzene ring are substituted by methyl, and has three isomers of ortho, meta and para, and industrially, the xylene refers to a mixture of the isomers; which can respectively generate phthalic acid, terephthalic acid, isophthalic acid and the like through oxygen oxidation.
Terephthalic acid is an important bulk chemical produced by air oxidation of meta-xylene (PX for short). In the prior art, the preparation process of terephthalic acid is that raw materials are in contact with oxygen in the air to generate oxidation reaction in a stirred reaction kettle by taking acetic acid as a solvent and cobalt, manganese and bromine as catalysts, and m-xylene is oxidized to produce terephthalic acid.
SUMMERY OF THE UTILITY MODEL
The utility model provides a control system for m-xylene oxidation production terephthalic acid for solve the too high problem of pressure among the reaction sequence.
The utility model provides a control system of m-xylene oxidation production terephthalic acid, include: the system comprises a slurry bed reactor, a first micro-interface generator, a second micro-interface generator, a condensing unit, a separating unit, a temperature control circulating pipeline, a crystallization filter and an intelligent control unit;
the slurry bed reactor is used as a reaction place for oxidizing the dimethylbenzene, an acetic acid solvent is filled in the slurry bed reactor, a pipeline is arranged above the slurry bed reactor and connected with the condensing unit, and a pipeline is arranged below the slurry bed reactor and connected with the crystallization filter;
the first micro-interface generator is arranged on a fixed plate in the slurry bed reactor and is used for enabling the liquid-phase separation materials from the separation unit and oxygen to form gas-liquid emulsion;
the second micro-interface generator is arranged in the slurry bed reactor and positioned below the first micro-interface generator and used for breaking bubbles from the gas inlet pipeline;
the temperature control circulating pipeline is arranged outside the slurry bed reactor, comprises a heat exchanger and a material pumping pump and is used for pumping liquid at the bottom of the slurry bed reactor into the liquid phase inlet of the second micro-interface generator so as to achieve the effects of controlling the temperature in the reactor and driving the liquid in the reactor to circulate;
the separation unit is used for carrying out gas-liquid separation on the materials from the condensation unit, discharging the separated gas-phase materials into a downstream tail gas treatment device, and discharging the discharged liquid-phase materials into the liquid-phase material inlet of the first micro-interface generator;
the intelligent control unit comprises a sensor, a controller and a central processing unit, the sensor transmits acquired electric signals to the central processing unit, the central processing unit processes and calculates data and then sends corresponding commands to the controller to achieve a control function, and the central processing unit uploads the acquired information to a network in real time so that a worker can monitor the working state of the system at any time through mobile equipment and remotely modify preset values of temperature and pressure in the processor.
Further, the acetic acid solvent in the slurry bed reactor accounted for 4/5 of the entire reactor volume.
Further, the fixed plate is disposed at a position of the total height 2/3 of the slurry bed reactor.
Further, a solvent inlet, a feed inlet and a catalyst inlet of the slurry bed reactor are all arranged between the first micro-interface generator and the second micro-interface generator.
Further, a gas inlet is connected with the gas phase inlet of the first micro-interface generator and the second micro-interface generator through a pipeline.
Further, the first micro-interface generator is a hydraulic micro-interface generator.
Further, the second micro-interface generator is a pneumatic micro-interface generator.
Further, the sensor includes:
at least one temperature sensor disposed in the slurry bed reactor to monitor a reaction temperature within the reactor;
at least one pressure sensor disposed in the slurry bed reactor to monitor a reaction pressure within the reactor;
at least one liquid level sensor disposed in the slurry bed reactor for monitoring a liquid level height within the reactor.
Further, the controller includes:
the first controller is arranged on the heat exchanger and used for controlling the working power of the heat exchanger;
the second controller is arranged on the material pumping pump and used for controlling the material pumping speed of the material pumping pump;
the first control valve is arranged on a pipeline connected with an air inlet and used for controlling the air inflow entering the slurry bed reactor;
and the second control valve is arranged on a pipeline connecting the slurry bed reactor and the crystallization filter and used for controlling the output state of the slurry bed reactor material.
Compared with the prior art, the utility model has the advantages of improving the mass transfer efficiency of gas-liquid two phases, reducing the reaction time and reducing the material consumption and energy consumption;
furthermore, a first micro-interface generator and a second micro-interface generator are arranged in the slurry bed reactor and break gas into micro-bubbles at the micron level, 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 gas stays in the reactor for a longer time, and the utilization rate of the oxygen is improved;
furthermore, a catalyst additive pipeline is arranged between the first micro-interface generator and the second micro-interface generator, and the catalyst is suspended in the reactor all the time when entering the slurry bed reactor under the influence of the floating action force of bubbles broken by the second micro-interface generator below, so that the catalytic efficiency is improved;
furthermore, a temperature control pipeline is arranged outside the slurry bed reactor, liquid-phase materials at the bottom of the reactor are pumped into the first 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 a catalyst is avoided, and the temperature control unit controls the temperature in the reactor by controlling the temperature of the liquid-phase materials flowing through, so that the reaction efficiency is ensured;
furthermore, an intelligent control unit is arranged in the whole reaction system, so that a worker can know the real-time situation of each data transmitted back by the sensor at any time through mobile equipment, and can realize accurate control of the temperature and the pressure in the whole slurry bed reactor by changing a preset value, thereby further improving the reaction efficiency.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention;
fig. 2 is a control flow chart according to an embodiment of the present invention.
Detailed Description
In order to make the objects and advantages of the invention more apparent, the invention is further described below with reference to the following embodiments; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element 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 otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected 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 specific situations.
Referring to fig. 1, a schematic structural diagram of the present invention for producing terephthalic acid by oxidizing meta-xylene, the system includes: the system comprises a slurry bed reactor 1, a first micro-interface generator 2, a solvent inlet 3, a feed inlet 4, a catalyst inlet 5, a second micro-interface generator 6, a condensing unit 7, a tail gas discharge outlet 8, a separation unit 9, a temperature control circulating pipeline 10, a gas inlet 11, a crystallization filter 12 and a solid product outlet 13.
With continued reference to fig. 1, the gas inlet 11 is connected by a conduit to the gas inlet of the first micro-interface generator 2 and to the second micro-interface generator 6; the first interface generator 2 is arranged on a fixing plate 21 positioned in the slurry bed reactor 1, and the micro-interface generator 6 is arranged in the slurry bed reactor 1 and positioned below the first interface generator 2; the temperature control circulating pipeline 10 comprises a heat exchanger 101 and a material pumping pump 102, is arranged outside the slurry bed reactor 1, and is used for pumping out the liquid phase material at the bottom of the slurry bed, and returning the liquid phase material to the reactor through a liquid inlet of the first micro-interface generator 2 after the temperature reduction treatment of the heat exchanger 101.
Continuing to refer to fig. 1, the gas phase outlet of the slurry bed reactor 1 is connected with the condensing unit 7, the condensing unit 7 is connected with the separating unit 9, and the liquid phase 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.
With continued reference to fig. 1, at least one temperature sensor 17 is provided in the slurry bed reactor 1 for monitoring the reaction temperature within the reactor; at least one pressure sensor 19 provided in the slurry bed reactor 1 to monitor the reaction pressure inside the reactor; at least one level sensor 18 disposed in the slurry bed reactor 1 for monitoring the level of liquid within the reactor; a first controller, which is arranged on the heat exchanger 101 and is used for controlling the working power of the heat exchanger 101; the second controller is arranged on the pumping pump 102 and used for controlling the pumping speed of the pumping pump 102; the first control valve 14 is arranged on a pipeline connected with the air inlet and used for controlling the air inflow entering the slurry bed reactor; and a second control valve 15 provided on a pipe connecting the slurry bed reactor 1 and the crystallization filter 12 for controlling the output state of the material of the slurry bed reactor 1.
Referring to fig. 1 and 2, the intelligent process of the present embodiment includes:
step 3, after a gas-phase product in the slurry bed reactor enters a condensing unit for condensation, the gas-phase product enters a separating unit for gas-liquid separation, a gas-phase material is discharged to a downstream tail gas treatment unit through a tail gas discharge port, and a liquid-phase material is discharged to a liquid-phase inlet of the first micro-interface generator;
step 4, monitoring the temperature of the reactor by a temperature sensor arranged in the slurry bed reactor, sending an electric signal to a central processing unit by the temperature sensor when the temperature is not matched with a preset value, sending a control command to the first controller and the second controller by the central processing unit, and realizing a temperature control function by adjusting the power of a heat exchanger and the speed of a material pumping pump; the pressure sensor arranged in the slurry bed reactor monitors the pressure of the reactor, when the pressure is not matched with a preset value, the pressure sensor sends an electric signal to the central processing unit, the central processing unit sends a control command to the first control valve, and the reaction rate and the reaction pressure are controlled by controlling the air inflow; the liquid level sensor arranged in the slurry bed reactor monitors the liquid level of the reactor, when the liquid level exceeds a preset value, the liquid level sensor sends an electric signal to the central processing unit, the central processing unit sends a control command to the second control valve, and the second control valve opens the valve to discharge redundant liquid-phase materials to the crystallization filter.
In this embodiment, the pressure sensor is a MIK-P310 pressure sensor manufactured by mike, the temperature sensor is a pt100 temperature sensor manufactured by meiaccuse, and the control valve is an electric control valve manufactured by australian, zhejiang.
The preset values for this example are shown in table 1:
TABLE 1
Preset value | Upper limit of | Lower limit of |
Reaction temperature (. degree. C.) in slurry bed reactor | 200 | 140 |
Reaction pressure intensity (MPa) in slurry bed reactor | 1.5 | 0.5 |
Oxidizing m-xylene as a raw material to prepare terephthalic acid, wherein the reaction pressure is 1.45MPa, and the mass ratio of m-xylene, acetic acid solvent and catalyst is 1: 3: 0.001; when the reaction is started, the acetic acid solvent and the m-xylene enter a slurry bed reactor to form a mixed solution, oxygen enters a second micro-interface generator and is smashed into micron-level bubbles, and the micron-level bubbles and the surrounding mixed solution form a gas-liquid emulsion; meanwhile, the catalyst enters the slurry bed reactor through a catalyst additive pipeline above the second micro-interface generator and is suspended in the slurry bed reactor under the upward floating action of the micron-sized bubbles crushed by the second micro-interface generator; the temperature control circulating unit extracts the liquid phase material at the bottom of the slurry bed reactor, the liquid phase material is heated or cooled to 150 ℃ by the heat exchanger and then is sent into the liquid phase inlet of the first micro-interface generator together with the liquid phase material separated from the separation unit, meanwhile, oxygen enters the gas phase inlet of the first micro-interface generator, the liquid phase material forms turbulence in the first micro-interface generator, and the entering oxygen is sucked in to form gas-liquid emulsion, so that the reaction rate is accelerated, and the reaction pressure is reduced.
The technical effects of the embodiment are as follows: the conversion rate of m-xylene is 97-99%, and the yield of terephthalic acid is 98%.
Claims (9)
1. A control system for the oxidation of meta-xylene to produce terephthalic acid, comprising: the system comprises a slurry bed reactor, a first micro-interface generator, a second micro-interface generator, a condensing unit, a separating unit, a temperature control circulating pipeline, a crystallization filter and an intelligent control unit;
the slurry bed reactor is used as a reaction place for oxidizing the dimethylbenzene, an acetic acid solvent is filled in the slurry bed reactor, a pipeline is arranged above the slurry bed reactor and connected with the condensing unit, and a pipeline is arranged below the slurry bed reactor and connected with the crystallization filter;
the first micro-interface generator is arranged on a fixed plate in the slurry bed reactor and is used for enabling the liquid-phase separation materials from the separation unit and oxygen to form gas-liquid emulsion;
the second micro-interface generator is arranged in the slurry bed reactor and positioned below the first micro-interface generator and used for breaking bubbles from the gas inlet pipeline;
the temperature control circulating pipeline is arranged outside the slurry bed reactor, comprises a heat exchanger and a material pumping pump and is used for pumping liquid at the bottom of the slurry bed reactor into the liquid phase inlet of the second micro-interface generator so as to achieve the effects of controlling the temperature in the reactor and driving the liquid in the reactor to circulate;
the separation unit is used for carrying out gas-liquid separation on the materials from the condensation unit, discharging the separated gas-phase materials into a downstream tail gas treatment device, and discharging the discharged liquid-phase materials into the liquid-phase material inlet of the first micro-interface generator;
the intelligent control unit comprises a sensor, a controller and a central processing unit, the sensor transmits acquired electric signals to the central processing unit, the central processing unit processes and calculates data and then sends corresponding commands to the controller to achieve a control function, and the central processing unit uploads the acquired information to a network in real time so that a worker can monitor the working state of the system at any time through mobile equipment and remotely modify preset values of temperature and pressure in the processor.
2. The control system for the oxidation of m-xylene to produce terephthalic acid according to claim 1, wherein the acetic acid solvent in said slurry bed reactor comprises 4/5 of the entire reactor volume.
3. The control system for the oxidation of m-xylene to produce terephthalic acid according to claim 1, characterized in that said fixed plate is disposed at the position of the total height 2/3 of said slurry bed reactor.
4. The control system for the oxidation of meta-xylene to produce terephthalic acid according to claim 1, characterized in that the solvent inlet, feed inlet and catalyst inlet of the slurry bed reactor are all disposed between the first and second micro-interfacial generators.
5. The control system for the production of terephthalic acid by the oxidation of metaxylene according to claim 1, wherein a gas inlet is connected to the gas phase inlet of said first micro-interface generator and said second micro-interface generator by a pipe.
6. The system for controlling the oxidation of meta-xylene to produce terephthalic acid according to any one of claims 1-5, wherein said first micro-interface generator is a hydraulic micro-interface generator.
7. The control system for the oxidation of meta-xylene to produce terephthalic acid according to any one of claims 1 to 5, wherein said second micro-interface generator is a pneumatic micro-interface generator.
8. The control system for the production of terephthalic acid by the oxidation of metaxylene according to any one of claims 1 to 5, characterized in that said sensor comprises:
at least one temperature sensor disposed in the slurry bed reactor to monitor a reaction temperature within the reactor;
at least one pressure sensor disposed in the slurry bed reactor to monitor a reaction pressure within the reactor;
at least one liquid level sensor disposed in the slurry bed reactor for monitoring a liquid level height within the reactor.
9. The control system for the production of terephthalic acid by the oxidation of metaxylene according to any one of claims 1 to 5, wherein said controller comprises:
the first controller is arranged on the heat exchanger and used for controlling the working power of the heat exchanger;
the second controller is arranged on the material pumping pump and used for controlling the material pumping speed of the material pumping pump;
the first control valve is arranged on a pipeline connected with an air inlet and used for controlling the air inflow entering the slurry bed reactor;
and the second control valve is arranged on a pipeline connecting the slurry bed reactor and the crystallization filter and used for controlling the output state of the slurry bed reactor material.
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CN201921498349.7U CN213078425U (en) | 2019-09-10 | 2019-09-10 | Control system for producing terephthalic acid by oxidizing m-xylene |
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