CN112479859A - Intelligent intensified reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation - Google Patents
Intelligent intensified reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation Download PDFInfo
- Publication number
- CN112479859A CN112479859A CN201910866980.6A CN201910866980A CN112479859A CN 112479859 A CN112479859 A CN 112479859A CN 201910866980 A CN201910866980 A CN 201910866980A CN 112479859 A CN112479859 A CN 112479859A
- Authority
- CN
- China
- Prior art keywords
- reaction
- carbonylation
- micro
- methanol
- carbon monoxide
- Prior art date
- Legal status (The legal status 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 status listed.)
- Withdrawn
Links
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 288
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 162
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 141
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 105
- 230000006315 carbonylation Effects 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 86
- 239000000047 product Substances 0.000 claims abstract description 72
- 238000001704 evaporation Methods 0.000 claims abstract description 42
- 230000008020 evaporation Effects 0.000 claims abstract description 42
- 238000000746 purification Methods 0.000 claims abstract description 23
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 21
- 238000012545 processing Methods 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims description 45
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 28
- 239000012071 phase Substances 0.000 claims description 27
- 230000018044 dehydration Effects 0.000 claims description 25
- 238000006297 dehydration reaction Methods 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 24
- 230000020335 dealkylation Effects 0.000 claims description 21
- 238000006900 dealkylation reaction Methods 0.000 claims description 21
- 238000003860 storage Methods 0.000 claims description 20
- 239000007791 liquid phase Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 238000011049 filling Methods 0.000 claims description 9
- 238000012546 transfer Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000010485 coping Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 ethylene acetaldehyde acetic acid Chemical compound 0.000 description 2
- 238000007701 flash-distillation Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000005805 hydroxylation reaction Methods 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- ZQRKXTKCZLIFIR-UHFFFAOYSA-N acetaldehyde;acetic acid;ethanol Chemical compound CCO.CC=O.CC(O)=O ZQRKXTKCZLIFIR-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/10—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide
- C07C51/12—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide on an oxygen-containing group in organic compounds, e.g. alcohols
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides an intelligent intensified reaction system and a process for preparing acetic acid by low-pressure low-temperature methanol carbonylation, which comprises the following steps: a feed unit to store and transport carbon monoxide and methanol; the reaction kettle is connected with the feeding unit and is used as a place for carbonylation reaction; the micro-interface generator is arranged in the reaction kettle and used for crushing the carbon monoxide into micro-bubbles with the diameter of micron level before the carbonylation reaction and then carrying out flash evaporation on the micro-bubbles; the device is connected with the reaction kettle and is used for carrying out flash evaporation treatment on the carbonylation reaction product; the product purification unit is connected with the flash tower and is used for processing and purifying flash products to finally obtain finished acetic acid; and the intelligent control unit is used for realizing the optimal control function. The invention provides an intelligent intensified reaction system and a process for preparing acetic acid by low-pressure low-temperature methanol carbonylation, which solve the problem of low reaction efficiency of the system in the prior art because carbon monoxide and methanol cannot be fully mixed in a carbonylation reaction kettle.
Description
Technical Field
The invention relates to the technical field of acetic acid preparation, in particular to an intelligent enhanced reaction system and process for preparing acetic acid by low-pressure low-temperature methanol carbonylation.
Background
Acetic acid is an important basic chemical raw material, and is one of important organic chemical products which develop rapidly in recent years. The industrial synthesis method of acetic acid mainly comprises an ethylene acetaldehyde acetic acid two-step method, an ethanol acetaldehyde acetic acid two-step method, an alkane and light oil oxidation method and a methanol carbonylation method. The methanol low pressure oxo process for the synthesis of acetic acid developed by Monsanto, USA has become the world's main production method for the production of acetic acid since the development and commissioning of the last 60 s of the 20 th century. The process adopts rhodium halide as a catalyst and methyl iodide as a promoter, and realizes the synthesis of acetic acid by methanol and carbon monoxide through carbonyl under the pressure of 28-30MPa and the temperature of 175-185 ℃.
Compared with the Monsanto process, the process adds a conversion reaction kettle, can convert an unstable rhodium complex into a complex with better thermal stability, adopts an evaporation process, improves the production capacity of a reactor, reduces energy consumption, adopts methanol as an absorbent for tail gas absorption, and has the advantages of good absorption effect, good product quality, small corrosion to equipment and the like.
However, in the case of producing acetic acid by using the conventional carbonylation reaction system, the carbonylation reaction is performed by directly introducing the methanol liquid and the carbon monoxide gas into the carbonylation reaction vessel, and the methanol liquid and the carbon monoxide gas are not sufficiently mixed in the carbonylation reaction vessel, so that the reaction efficiency of the system is lowered.
Disclosure of Invention
In view of the above, the invention provides an intelligent enhanced reaction system and process for preparing acetic acid by carbonylation of methanol at low pressure and low temperature, so as to solve the problem that in the prior art, the reaction efficiency of the system is reduced because carbon monoxide and methanol cannot be fully mixed in a carbonylation reaction kettle.
The technical purpose of the invention is realized by the following technical scheme.
An intelligent enhanced reaction system for preparing acetic acid by low-pressure low-temperature methanol carbonylation comprises:
a feed unit to store and transport carbon monoxide and methanol;
the reaction kettle is connected with the feeding unit, is used for receiving methanol and serves as a place for carbonylation reaction;
the micro-interface generator is arranged in the reaction kettle, is connected with the feeding unit, and is used for receiving the carbon monoxide and crushing the carbon monoxide into micro-bubbles with the diameter of micron level before the carbonylation reaction so as to increase the mass transfer area of a phase boundary between the carbon monoxide and the methanol in the carbonylation reaction process and enhance the carbonylation reaction efficiency;
the flash tower is connected with the reaction kettle and is used for carrying out flash evaporation treatment on the carbonylation reaction product and circulating the catalyst in the flash evaporation product to the interior of the reaction kettle for the carbonylation reaction in the reaction kettle again;
the product purification unit is connected with the flash tower and is used for processing and purifying flash products to finally obtain finished acetic acid;
the intelligent control unit comprises sensors and controllers which are respectively arranged on the designated equipment, and cloud processors which are arranged outside the system and are respectively connected with the sensors and the controllers, wherein the sensors transmit acquired electric signals to the cloud processors, the cloud processors screen and compare reaction parameters returned by the sensors in a cloud database, and send corresponding commands to the controllers after an optimal control method is screened out, so that the optimal control function is realized.
Further, the micro-interface generator breaks the hydrogen gas into micro-bubbles having a diameter of a micrometer scale by converting pressure energy of the gas and/or kinetic energy of the liquid into bubble surface energy and transferring the same to the hydrogen gas bubbles.
Further, the micro-interface generator is selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
Further, the micro-bubbles of the micron level are micro-bubbles with the diameter of more than or equal to 1 μm and less than 1 mm.
Further, the feed unit comprises:
a liquid phase storage tank connected with the reaction tank and used for storing and conveying the methanol solution,
and the gas phase feeding pipeline is connected with the micro interface generator and is externally connected with a gas source and used for conveying the carbon monoxide to the micro interface generator.
Further, be provided with the circulating pump between liquid phase storage jar and the reation kettle for with the inside methyl alcohol of liquid phase storage jar inside with appointed speed transport to reation kettle inside.
Further, the product purification unit comprises:
the dehydrogenation tower is connected with the flash tower and is used for carrying out dehydrogenation treatment on the flash product;
the dehydration tower is connected with the dehydrogenation tower and is used for dehydrating the dehydrogenation product;
and the dealkylation tower is connected with the dehydration tower and is used for carrying out dealkylation treatment on the dehydration product.
Further, the intelligent control unit includes:
the reaction sensor is arranged in the reaction kettle and used for detecting the reaction pressure in the reaction kettle in real time;
the circulating controller is arranged on the circulating pump and used for controlling the reaction pressure of the reaction kettle by adjusting the power of the circulating pump to change the flow of the materials in the system;
and the cloud processor is arranged outside the system, can be respectively connected with the reaction sensor and the circulation controller, and is used for receiving the signal sent by the reaction sensor and sending a control signal to the circulation controller.
In another aspect, the present invention provides an intelligent enhanced reaction process for preparing acetic acid by low-pressure low-temperature methanol carbonylation, comprising:
filling methanol and a catalyst into a methanol storage tank, connecting a carbon monoxide feeding pipeline with a carbon monoxide gas source, starting a system, conveying the methanol and the catalyst into a reaction kettle, and simultaneously conveying the carbon monoxide into a micro-interface generator through the carbon monoxide feeding pipeline;
the micro-interface generator breaks carbon monoxide into micro-bubbles with micron scale, and releases the micro-bubbles into the reaction kettle so as to increase the mass transfer area of a phase boundary between the carbon monoxide and the methanol in the carbonylation reaction process, so that the carbon monoxide is fully contacted with the methanol in the micro-bubble state, and the carbonylation reaction is carried out;
conveying the carbonylation reaction product to the inside of a flash tower for flash evaporation treatment, circulating the catalyst obtained by flash evaporation to the inside of a reaction kettle, reusing the catalyst in the carbonylation reaction inside the reaction kettle, and conveying other products obtained by flash evaporation to a product purification unit;
the product purification unit is used for sequentially carrying out dehydrogenation, dehydration and dealkylation on other products obtained by flash evaporation to finally obtain finished acetic acid;
in the system operation process, the reaction sensor can detect the pressure in the reaction kettle, the reaction sensor can send the detected numerical value to the cloud processor in an electric signal mode after the detection is finished, when the detection value exceeds a preset range, the cloud processor can screen and compare in the cloud database to select an optimal coping scheme, and the circulating controller is controlled to adjust the circulating pump to adjust the reaction pressure in the system.
Further, the carbonylation reaction temperature is 130-150 ℃, and the reaction pressure is 0.1-0.3 MPa.
In summary, the intelligent enhanced reaction system and process for preparing acetic acid by carbonylation of methanol at low pressure and low temperature provided by the invention have the beneficial effects that the micro-interface generator connected with the gas-phase feeding pipeline is arranged in the reaction kettle, so that before the carbonylation reaction of carbon monoxide and methanol, the micro-interface generator breaks the carbon monoxide into micro-bubbles with the diameter of more than or equal to 1 μm and less than 1mm, the carbon monoxide is contacted with the methanol in the micro-bubble state, the mass transfer area of the phase boundary between the carbon monoxide and the methanol in the carbonylation reaction process is increased, and the carbon monoxide and the methanol are fully mixed and then subjected to the carbonylation reaction, thereby solving the problem that the reaction efficiency of the system is reduced because the carbon monoxide and the methanol cannot be fully mixed in the carbonylation reaction kettle in the prior art.
Furthermore, the intelligent control unit is arranged in the system, can detect various parameters in the operation of the system through the sensor, performs screening comparison in the cloud database through the cloud processor, selects the optimal scheme to send an instruction to the controller so that the controller performs corresponding operation on the specified equipment, can complete automatic learning and regulation of the system through the cloud processor, improves the safety factor of the system, and further improves the operation efficiency of the system.
Especially, be provided with the circulating pump between liquid phase storage jar and the reation kettle, when this system operation, the circulating pump can provide power for the transportation of methyl alcohol, makes methyl alcohol can carry to reation kettle with appointed speed, has improved the operating efficiency of this system.
Particularly, in the system, the carbonylation reaction product can be subjected to flash evaporation treatment by the flash evaporation tower, and the catalyst in the flash evaporation product is circulated to the inside of the reaction kettle and is used for the carbonylation reaction in the reaction kettle again, so that the production cost is further saved.
Particularly, the product purification unit is provided with a dehydrogenation tower, a dehydration tower and a dealkylation tower, so that the flash evaporation product can obtain high-purity finished product ethylene after dehydrogenation, dehydration and dealkylation.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic structural diagram of an intelligent enhanced reaction system and process for preparing acetic acid by low-pressure and low-temperature methanol carbonylation according to an embodiment of the present invention;
fig. 2 is a flow chart of an intelligent enhanced reaction system and process for preparing acetic acid by low-pressure low-temperature methanol carbonylation according to an embodiment of the present invention.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the 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 in a specific orientation, and be operated, 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 meanings 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, an intelligent enhanced reaction system for preparing acetic acid by low-pressure and low-temperature methanol carbonylation according to an embodiment of the present invention includes: a feed unit to store and transport carbon monoxide and methanol; a reaction kettle 3 connected with the feeding unit, for receiving methanol and serving as a place for carbonylation reaction; the micro-interface generator 2 is arranged in the reaction kettle 3, is connected with the feeding unit, and is used for receiving the carbon monoxide and crushing the carbon monoxide into micro-bubbles with the diameter of more than or equal to 1 micrometer and less than 1mm before the carbonylation reaction so as to increase the mass transfer area of a phase boundary between the carbon monoxide and the methanol in the carbonylation reaction process and enhance the efficiency of the carbonylation reaction; a flash column 4; the device is connected with the reaction kettle 3 and is used for carrying out flash evaporation treatment on the carbonylation reaction product, and circulating the catalyst in the flash evaporation product to the interior of the reaction kettle 3 for the carbonylation reaction in the reaction kettle 3 again; the product purification unit is connected with the flash tower 4 and is used for processing and purifying flash products to finally obtain finished acetic acid; the intelligent control unit comprises sensors and controllers which are respectively arranged on the designated equipment, and cloud processors which are arranged outside the system and are respectively connected with the sensors and the controllers, wherein the sensors transmit acquired electric signals to the cloud processors, the cloud processors screen and compare reaction parameters returned by the sensors in a cloud database, and send corresponding commands to the controllers after an optimal control method is screened out, so that the optimal control function is realized.
Preferably, the micro-interface generator 2 converts pressure energy of gas and/or kinetic energy of liquid into surface energy of bubbles and transmits the surface energy to the bubbles, so that the bubbles are broken into micro-bubbles with the diameter of more than or equal to 1 μm and less than 1mm, and the micro-bubbles are divided into a pneumatic micro-interface generator 2, a hydraulic micro-interface generator 2 and a gas-liquid linkage micro-interface generator 2 according to an energy input mode or a gas-liquid ratio, wherein the pneumatic micro-interface generator 2 is driven by gas, and the input gas quantity is far greater than the liquid quantity; the hydraulic micro-interface generator 2 is driven by liquid, and the input air quantity is generally smaller than the liquid quantity; the gas-liquid linkage type micro-interface generator 2 is driven by gas and liquid at the same time, and the input gas quantity is close to the liquid quantity. The micro-interface generator 2 is one or more of a pneumatic micro-interface generator 2, a hydraulic micro-interface generator 2 and a gas-liquid linkage micro-interface generator 2.
Referring to fig. 1, the feed unit includes: the gas-phase feeding pipeline 11 is in a shape of a slender round pipe, one end of the gas-phase feeding pipeline is externally connected with a gas source, and the other end of the gas-phase feeding pipeline is connected with the micro-interface generator 2 and is used for receiving carbon monoxide and conveying the carbon monoxide to the micro-interface generator 2; liquid phase storage jar 12 is short thick round tank form, its with reation kettle 3 connects for save methyl alcohol, be provided with between liquid phase storage jar 12 and reation kettle 3, be used for carrying the inside methyl alcohol of liquid phase storage jar 12 to reation kettle 3 inside circulating pump 13. When the system is used, methanol and corresponding catalysts are filled in a liquid-phase storage tank 12, a gas-phase feeding pipeline 11 is connected with a gas source of carbon monoxide, the system is started, a circulating pump 13 conveys the methanol and the catalysts to the inside of a reaction kettle 3, meanwhile, the carbon monoxide is conveyed to the inside of a micro-interface generator 2 through the gas-phase feeding pipeline 11, the micro-interface generator 2 breaks the carbon monoxide into micro bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, and the micro bubbles are released to the inside of the reaction kettle 3 to increase the phase boundary mass transfer area between the carbon monoxide and the methanol in a carbonylation reaction process, so that the carbon monoxide is fully contacted with the methanol in the micro-bubble state and is subjected to carbonylation reaction, waste gas generated in the carbonylation reaction is discharged from the top end of the reaction kettle 3, and a carbonylation reaction product.
The product purification unit, comprising: a dehydrogenation tower 51 connected with the flash tower 4 and used for carrying out dehydrogenation treatment on the flash product; a dehydration column 52 connected to the dehydrogenation column 51, for dehydrating the dehydrogenation product; and the dealkylation tower 53 is connected with the dehydration tower 52 and is used for dealkylating the dehydration product to finally obtain the finished product acetic acid. When the flash evaporation product is conveyed to the product purification unit, the flash evaporation product is subjected to corresponding dehydrogenation, dehydration and dealkylation sequentially through the dehydrogenation tower 51, the dehydration tower 52 and the dealkylation tower 53 to finally obtain finished product acetic acid, the acetic acid is collected, and other components generated in the reaction process are removed from the system.
The intelligent control unit comprises: the reaction sensor 61 is arranged in the reaction kettle 3 and used for detecting the reaction pressure in the reaction kettle in real time; the circulating controller 62 is arranged on the circulating pump 13 and used for changing the flow of materials in the system by adjusting the power of the circulating pump so as to control the reaction pressure of the reaction kettle; and the cloud processor is arranged outside the system and can be respectively connected with the reaction sensor 61 and the circulation controller 62, and is used for receiving the signal sent by the reaction sensor 61 and sending a control signal to the circulation controller 62. When the reaction kettle 3 is in operation, the reaction sensor 61 detects the pressure in the reaction kettle 3, and transmits the detected result to the cloud processing system, when the detected value exceeds a preset pressure range, the cloud processor searches cloud data and screens an optimal scheme, and sends a control signal to the circulation controller 62, and after the circulation controller 62 receives the control signal, the power of the circulation pump is adjusted to control the pressure in the reaction kettle 3.
According to the intelligent enhanced reaction system and the process for preparing acetic acid by carbonylation of methanol at low pressure and low temperature, the micro-interface generator 2 connected with the gas-phase feeding pipeline 11 is arranged in the reaction kettle 3, so that before carbonylation of carbon monoxide and methanol, the carbon monoxide is crushed into micro bubbles with the diameter of more than or equal to 1 mu m and less than 1mm by the micro-interface generator 2, the carbon monoxide is contacted with the methanol in a micro bubble state, the phase boundary mass transfer area between the carbon monoxide and the methanol in the carbonylation reaction process is increased, and the carbon monoxide and the methanol are fully mixed and then subjected to carbonylation reaction, and the problem that in the prior art, the reaction efficiency of the system is reduced because the carbon monoxide and the methanol cannot be fully mixed in the carbonylation reaction kettle 3 is solved.
The intelligent control unit detects various parameters in the operation of the system through the sensor, the cloud processor performs screening comparison in the cloud database, the optimal scheme is selected to send an instruction to the controller so that the controller performs corresponding operation on the specified equipment, and the cloud processor is used to complete automatic learning and regulation of the system, improve the safety coefficient of the system and further improve the operation efficiency of the system.
The specific method and effect of the system of the present invention will be further described with reference to fig. 1.
An intelligent enhanced reaction process for preparing acetic acid by low-pressure low-temperature methanol carbonylation is characterized by comprising the following steps:
filling methanol and a catalyst into a methanol storage tank, connecting a carbon monoxide feeding pipeline with a carbon monoxide gas source, starting a system, conveying the methanol and the catalyst into a reaction kettle 3, and simultaneously conveying the carbon monoxide into a micro-interface generator 2 through the carbon monoxide feeding pipeline;
the micro-interface generator 2 breaks carbon monoxide into micro-bubbles with micron scale, and releases the micro-bubbles into the reaction kettle 3, so as to increase the phase boundary mass transfer area between the carbon monoxide and the methanol in the hydroxylation reaction process, so that the carbon monoxide is fully contacted with the methanol in the micro-bubble state, and hydroxylation reaction is carried out;
conveying the carbonylation reaction product to the inside of a flash tower 4 for flash evaporation treatment, circulating the catalyst obtained by flash evaporation to the inside of a reaction kettle 3 for carbonylation reaction in the reaction kettle 3 again, and conveying other products obtained by flash evaporation to a product purification unit;
the product purification unit is used for sequentially carrying out dehydrogenation, dehydration and dealkylation on other products obtained by flash evaporation to finally obtain finished acetic acid;
in the system operation process, the reaction sensor can detect the pressure in the reaction kettle, the reaction sensor can send the detected numerical value to the cloud processor in an electric signal mode after the detection is finished, when the detection value exceeds a preset range, the cloud processor can screen and compare in the cloud database to select an optimal coping scheme, and the circulating controller is controlled to adjust the circulating pump to adjust the reaction pressure in the system.
Preferably, the carbonylation reaction temperature is 130-150 ℃, and the carbonylation reaction pressure is 0.1-0.3 MPa.
In order to further verify the processing method provided by the invention, the beneficial effects of the invention are further illustrated by combining the examples and the comparative examples. Meanwhile, in the present embodiment, the kind of the catalyst is not particularly limited, and may be one or a combination of several kinds of rhodium-based catalyst, iridium-based catalyst, nickel-based catalyst, cobalt-based catalyst, and tungsten-based catalyst, as long as the strengthening reaction can be smoothly performed
Example 1
Filling sufficient methanol and a catalyst in a corresponding proportion into a liquid-phase storage tank 12, connecting a gas-phase feed pipeline 11 with a gas source containing 200L of carbon monoxide, starting a system, setting the temperature of the system at 130 ℃ and the pressure at 0.1MPa, conveying the methanol and the catalyst into a reaction kettle 3, and conveying the carbon monoxide into a micro-interface generator 2 through the gas-phase feed pipeline 11;
And (3) conveying the carbonylation reaction product to a flash tower 4, carrying out flash evaporation treatment on the carbonylation reaction product, circulating the catalyst in the flash evaporation product to the inside of the reaction kettle 3 for the carbonylation reaction inside the reaction kettle 3 again after the flash evaporation is finished, and conveying other products except the catalyst to a product purification unit.
The flash evaporation product conveyed to the product purification unit is subjected to corresponding dehydrogenation, dehydration and dealkylation sequentially through a dehydrogenation tower 51, a dehydration tower 52 and a dealkylation tower 53, so that a finished product of acetic acid is finally obtained, the acetic acid is collected, and other components generated in the reaction process are removed from the system. The acetic acid production was monitored and the carbon monoxide conversion was calculated to be 91%.
Example 2
Filling sufficient methanol and a catalyst in a corresponding proportion into a liquid-phase storage tank 12, connecting a gas-phase feed pipeline 11 with a gas source containing 200L of carbon monoxide, starting a system, setting the temperature of the system to be 140 ℃ and the pressure to be 0.2MPa, conveying the methanol and the catalyst into a reaction kettle 3, and conveying the carbon monoxide into a micro-interface generator 2 through the gas-phase feed pipeline 11;
And (3) conveying the carbonylation reaction product to a flash tower 4, carrying out flash evaporation treatment on the carbonylation reaction product, circulating the catalyst in the flash evaporation product to the inside of the reaction kettle 3 for the carbonylation reaction inside the reaction kettle 3 again after the flash evaporation is finished, and conveying other products except the catalyst to a product purification unit.
The flash evaporation product conveyed to the product purification unit is subjected to corresponding dehydrogenation, dehydration and dealkylation sequentially through a dehydrogenation tower 51, a dehydration tower 52 and a dealkylation tower 53, so that a finished product of acetic acid is finally obtained, the acetic acid is collected, and other components generated in the reaction process are removed from the system. The acetic acid production was monitored and the carbon monoxide conversion was calculated to be 94%.
Example 3
Filling sufficient methanol and a catalyst in a corresponding proportion into a liquid-phase storage tank 12, connecting a gas-phase feed pipeline 11 with a gas source containing 200L of carbon monoxide, starting a system, setting the temperature of the system at 150 ℃ and the pressure at 0.3MPa, conveying the methanol and the catalyst into a reaction kettle 3, and conveying the carbon monoxide into a micro-interface generator 2 through the gas-phase feed pipeline 11;
And (3) conveying the carbonylation reaction product to a flash tower 4, carrying out flash evaporation treatment on the carbonylation reaction product, circulating the catalyst in the flash evaporation product to the inside of the reaction kettle 3 for the carbonylation reaction inside the reaction kettle 3 again after the flash evaporation is finished, and conveying other products except the catalyst to a product purification unit.
The flash evaporation product conveyed to the product purification unit is subjected to corresponding dehydrogenation, dehydration and dealkylation sequentially through a dehydrogenation tower 51, a dehydration tower 52 and a dealkylation tower 53, so that a finished product of acetic acid is finally obtained, the acetic acid is collected, and other components generated in the reaction process are removed from the system. The acetic acid production was monitored and the carbon monoxide conversion was calculated to be 96%.
Comparative example 1
Filling sufficient methanol and a catalyst in a corresponding proportion into a liquid-phase storage tank 12, connecting a gas-phase feed pipeline 11 with a gas source containing 200L of carbon monoxide, starting a system, setting the temperature of the system at 130 ℃ and the pressure at 0.1MPa, conveying the methanol and the catalyst into a reaction kettle 3, and introducing the carbon monoxide into the reaction kettle 3 to carry out carbonylation reaction;
and (3) sequentially conveying the carbonylation reaction product to a flash tower 4, a dehydrogenation tower 51, a dehydration tower 52 and a dealkylation tower 53 to finally obtain a finished product of ethanol, detecting the yield of acetic acid, and calculating the conversion rate of carbon monoxide to be 81%.
Comparative example 2
Filling sufficient methanol and a catalyst in a corresponding proportion into a liquid-phase storage tank 12, connecting a gas-phase feed pipeline 11 with a gas source containing 200L of carbon monoxide, starting a system, setting the temperature of the system to be 140 ℃ and the pressure to be 0.2MPa, conveying the methanol and the catalyst into a reaction kettle 3, and introducing the carbon monoxide into the reaction kettle 3 to carry out carbonylation reaction;
and (3) sequentially conveying the carbonylation reaction product to a flash tower 4, a dehydrogenation tower 51, a dehydration tower 52 and a dealkylation tower 53 to finally obtain a finished product of ethanol, detecting the yield of acetic acid, and calculating the conversion rate of carbon monoxide to be 85%.
Comparative example 3
Filling sufficient methanol and a catalyst in a corresponding proportion into a liquid-phase storage tank 12, connecting a gas-phase feed pipeline 11 with a gas source containing 200L of carbon monoxide, starting a system, setting the temperature of the system at 150 ℃ and the pressure at 0.3MPa, conveying the methanol and the catalyst into a reaction kettle 3, and introducing the carbon monoxide into the reaction kettle 3 to carry out carbonylation reaction;
and (3) sequentially conveying the carbonylation reaction product to a flash tower 4, a dehydrogenation tower 51, a dehydration tower 52 and a dealkylation tower 53 to finally obtain a finished product of ethanol, detecting the yield of acetic acid, and calculating the conversion rate of carbon monoxide to be 89%.
In view of the above, the intelligent enhanced reaction system and process for preparing acetic acid by low-pressure and low-temperature methanol carbonylation provided by the invention solve the problem that in the prior art, the reaction efficiency of the system is reduced because carbon monoxide and methanol cannot be fully mixed in the carbonylation reaction kettle 3.
The above-mentioned embodiments are merely illustrative and not restrictive, and those skilled in the art can modify the embodiments without inventive contribution as required after reading this specification, but only fall within the scope of the claims of the present invention.
Claims (10)
1. An intelligent enhanced reaction system for preparing acetic acid by low-pressure low-temperature methanol carbonylation is characterized by comprising:
a feed unit to store and transport carbon monoxide and methanol;
the reaction kettle is connected with the feeding unit, is used for receiving methanol and serves as a place for carbonylation reaction;
the micro-interface generator is arranged in the reaction kettle, is connected with the feeding unit, and is used for receiving the carbon monoxide and crushing the carbon monoxide into micro-bubbles with the diameter of micron level before the carbonylation reaction so as to increase the mass transfer area of a phase boundary between the carbon monoxide and the methanol in the carbonylation reaction process and enhance the carbonylation reaction efficiency;
the flash tower is connected with the reaction kettle and is used for carrying out flash evaporation treatment on the carbonylation reaction product and circulating the catalyst in the flash evaporation product to the interior of the reaction kettle for the carbonylation reaction in the reaction kettle again;
the product purification unit is connected with the flash tower and is used for processing and purifying flash products to finally obtain finished acetic acid;
the intelligent control unit comprises sensors and controllers which are respectively arranged on the designated equipment, and cloud processors which are arranged outside the system and are respectively connected with the sensors and the controllers, wherein the sensors transmit acquired electric signals to the cloud processors, the cloud processors screen and compare reaction parameters returned by the sensors in a cloud database, and send corresponding commands to the controllers after an optimal control method is screened out, so that the optimal control function is realized.
2. The intelligent enhanced reaction system for the low pressure and low temperature methanol carbonylation to produce acetic acid as claimed in claim 1, wherein the micro-interface generator breaks the hydrogen gas into micro-bubbles with a diameter of micron level by converting the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubbles and transmitting the surface energy to the hydrogen gas bubbles.
3. The intelligent enhanced reaction system for preparing acetic acid through low-pressure low-temperature methanol carbonylation according to claim 1, wherein the micro-interface generator is one or more selected from a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
4. The intelligent intensified reaction system for preparing acetic acid through low-pressure low-temperature methanol carbonylation according to claim 1, wherein the micro-bubbles with a size of 1 μm or more and less than 1mm in diameter.
5. The intelligent, enhanced reaction system for the low pressure, low temperature methanol carbonylation to produce acetic acid of claim 1 wherein the feed unit comprises:
a liquid phase storage tank connected with the reaction tank and used for storing and conveying the methanol solution,
and the gas phase feeding pipeline is connected with the micro interface generator and is externally connected with a gas source and used for conveying the carbon monoxide to the micro interface generator.
6. The intelligent intensified reaction system for preparing acetic acid through low-pressure low-temperature methanol carbonylation according to claim 5, characterized in that a circulating pump is arranged between the liquid-phase storage tank and the reaction kettle and used for conveying the methanol in the liquid-phase storage tank to the reaction kettle at a specified speed.
7. The intelligent, enhanced reaction system for the low pressure, low temperature methanol carbonylation to produce acetic acid of claim 6 wherein the product purification unit comprises:
the dehydrogenation tower is connected with the flash tower and is used for carrying out dehydrogenation treatment on the flash product;
the dehydration tower is connected with the dehydrogenation tower and is used for dehydrating the dehydrogenation product;
and the dealkylation tower is connected with the dehydration tower and is used for carrying out dealkylation treatment on the dehydration product.
8. The intelligent enhanced reaction system for the low pressure low temperature methanol carbonylation to produce acetic acid of claim 6 wherein said intelligent control unit comprises:
the reaction sensor is arranged in the reaction kettle and used for detecting the reaction pressure in the reaction kettle in real time;
the circulating controller is arranged on the circulating pump and used for controlling the reaction pressure of the reaction kettle by adjusting the power of the circulating pump to change the flow of the materials in the system;
and the cloud processor is arranged outside the system, can be respectively connected with the reaction sensor and the circulation controller, and is used for receiving the signal sent by the reaction sensor and sending a control signal to the circulation controller.
9. An intelligent enhanced reaction process for preparing acetic acid by low-pressure low-temperature methanol carbonylation is characterized by comprising the following steps:
filling methanol and a catalyst into a methanol storage tank, connecting a carbon monoxide feeding pipeline with a carbon monoxide gas source, starting a system, conveying the methanol and the catalyst into a reaction kettle, and simultaneously conveying the carbon monoxide into a micro-interface generator through the carbon monoxide feeding pipeline;
the micro-interface generator breaks carbon monoxide into micro-bubbles with micron scale, and releases the micro-bubbles into the reaction kettle so as to increase the mass transfer area of a phase boundary between the carbon monoxide and the methanol in the carbonylation reaction process, so that the carbon monoxide is fully contacted with the methanol in the micro-bubble state, and the carbonylation reaction is carried out;
conveying the carbonylation reaction product to the inside of a flash tower for flash evaporation treatment, circulating the catalyst obtained by flash evaporation to the inside of a reaction kettle, reusing the catalyst in the carbonylation reaction inside the reaction kettle, and conveying other products obtained by flash evaporation to a product purification unit;
and the product purification unit is used for sequentially carrying out dehydrogenation, dehydration and dealkylation on other products obtained by flash evaporation to finally obtain the finished product acetic acid.
10. The intelligent enhanced reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation as claimed in claim 9, wherein the carbonylation reaction temperature is 130-150 ℃ and the reaction pressure is 0.1-0.3 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910866980.6A CN112479859A (en) | 2019-09-12 | 2019-09-12 | Intelligent intensified reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910866980.6A CN112479859A (en) | 2019-09-12 | 2019-09-12 | Intelligent intensified reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112479859A true CN112479859A (en) | 2021-03-12 |
Family
ID=74919992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910866980.6A Withdrawn CN112479859A (en) | 2019-09-12 | 2019-09-12 | Intelligent intensified reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112479859A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115591497A (en) * | 2022-10-26 | 2023-01-13 | 西南化工研究设计院有限公司（Cn） | Control system suitable for reactor temperature of low-pressure oxo-synthesis acetic acid device |
-
2019
- 2019-09-12 CN CN201910866980.6A patent/CN112479859A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115591497A (en) * | 2022-10-26 | 2023-01-13 | 西南化工研究设计院有限公司（Cn） | Control system suitable for reactor temperature of low-pressure oxo-synthesis acetic acid device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111362792A (en) | Enhanced reaction system and process for preparing acetic acid by methanol carbonylation | |
| CN105112100B (en) | Continuous production technique of chlorinated paraffin | |
| CN109534999B (en) | Synthesis process and device of dimethyl carbonate | |
| EP3519379A1 (en) | Method for acid treatment conditioning of a catalyst in the production of glycols | |
| CN111574345A (en) | Intelligent strengthening reaction system and process for built-in micro-interface unit for producing PTA (purified terephthalic acid) by PX (para-xylene) | |
| CN112479859A (en) | Intelligent intensified reaction system and process for preparing acetic acid through low-pressure low-temperature methanol carbonylation | |
| CN106928021A (en) | A kind of method of preparing ethylene glycol by using dimethyl oxalate plus hydrogen | |
| CN113480421B (en) | System and method for preparing succinic acid by maleic anhydride hydrogenation | |
| CN114456131A (en) | Tetrahydrofuran production system and preparation method | |
| CN102557932A (en) | Method for producing isobutyl acetate | |
| CN101402624B (en) | Method for producing trimellitic anhydride with pseudocumene liquid phase air segmenting hydrocarbonylation | |
| CN103664530A (en) | Method for coproducing cyclohexanol and ethanol | |
| CN101659588A (en) | Method and device of combined process for producing ethylene by ethanol dehydration and catalytic cracking | |
| CN103880598B (en) | A kind of method of coproduction hexalin and ethanol and device | |
| CN107628929B (en) | Production process for preparing 1, 2-propylene glycol by glycerol hydrogenolysis | |
| CN102010321A (en) | Process for continuously producing isobutyric acid | |
| CN211123731U (en) | Intelligent control reaction system for preparing ethylene glycol based on ethylene hydration method | |
| CN213506652U (en) | Enhanced carbonylation reaction system | |
| CN112479882A (en) | Reaction system and process for synthesizing dimethyl carbonate by liquid-phase oxidative carbonylation of methanol | |
| CN112479857A (en) | Low-pressure low-temperature methanol carbonylation enhanced reaction system and process for preparing acetic acid | |
| CN108658756B (en) | Method for preparing dichloroacetic acid by selective dechlorination of trichloroacetic acid | |
| CN112574021A (en) | Enhanced carbonylation reaction system and process | |
| CN102276453A (en) | Method for preparing isobomyl acetate through camphene esterification | |
| CN212120009U (en) | Etherification-free intelligent system for preparing propylene oxide by intensified propylene epoxidation | |
| CN112759505B (en) | Method and system for preparing ethylene glycol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210312 |
|
| WW01 | Invention patent application withdrawn after publication |