CN212119940U - Methanol carbonylation enhanced reaction system with aldehyde recovery function - Google Patents
Methanol carbonylation enhanced reaction system with aldehyde recovery function Download PDFInfo
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- CN212119940U CN212119940U CN201921521687.8U CN201921521687U CN212119940U CN 212119940 U CN212119940 U CN 212119940U CN 201921521687 U CN201921521687 U CN 201921521687U CN 212119940 U CN212119940 U CN 212119940U
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 270
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 38
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 title claims abstract description 36
- 238000011084 recovery Methods 0.000 title claims abstract description 29
- 230000006315 carbonylation Effects 0.000 title claims abstract description 24
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 83
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 70
- 230000003197 catalytic effect Effects 0.000 claims abstract description 26
- 238000012546 transfer Methods 0.000 claims abstract description 25
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 186
- 229920001744 Polyaldehyde Polymers 0.000 claims description 63
- 239000003054 catalyst Substances 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 21
- 238000007670 refining Methods 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 16
- 238000004891 communication Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
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- 230000008569 process Effects 0.000 description 25
- 239000006227 byproduct Substances 0.000 description 15
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- 230000005540 biological transmission Effects 0.000 description 9
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 230000009471 action Effects 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 6
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 235000019260 propionic acid Nutrition 0.000 description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910021604 Rhodium(III) chloride Inorganic materials 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
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- 239000013064 chemical raw material Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
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- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 1
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Abstract
The utility model relates to a reaction system is reinforceed in methyl alcohol carbonylation with aldehyde is retrieved, include: a reactor, a micro-interface generator, an aldehyde recovery unit, and the like. The utility model discloses a broken methyl alcohol gas and carbon monoxide gas make it form micron order bubble of micron yardstick, make micron order bubble and catalysis liquid mix and form gas-liquid mixture to increase the gas-liquid diphasic interfacial area, and reach the effect of strengthening the mass transfer in lower predetermined operating condition scope; meanwhile, the micron-sized bubbles can be fully mixed with the catalytic liquid to form a gas-liquid mixture, and the gas-liquid mixture can ensure that the catalytic liquid in the system can be fully contacted with methanol gas and carbon monoxide gas by fully mixing the gas phase and the liquid phase, so that the reaction efficiency of the system is effectively improved.
Description
Technical Field
The utility model relates to an acetic acid preparation technical field especially relates to a reaction system is reinforceed in methyl alcohol carbonylation with aldehyde is retrieved.
Background
Acetic acid is an important basic organic chemical raw material, and main raw materials such as chloroacetic acid, vinyl acetate monomers, polyvinyl alcohol, terephthalic acid, acetate fibers, metal acetate and the like are synthesized by acetic acid, so that the acetic acid has wide application in various aspects such as pesticides, medicines, dyes, adhesives, organic solvents and the like along with scientific development.
The methanol carbonylation method uses methanol and carbon monoxide as raw materials to synthesize acetic acid through carbonylation, and has the main advantages of less by-products, diversified raw material routes, coal coke, natural gas and heavy oil as basic raw materials, particular application to coal chemical industry, less three wastes, long service life, less consumption, high catalyst activity and easy treatment.
The methanol carbonylation method can be divided into a low pressure method and a high pressure method according to the synthesis pressure, the high pressure method is to synthesize the acetic acid by carbonylation by taking iodine as a cocatalyst and cobalt carbonyl as a catalyst under the conditions of the temperature of 250 ℃ and the pressure of 63.74Mpa, the yield is between 88 and 90 percent, and the low pressure method is to synthesize the acetic acid by carbonylation by taking monoiodomethane as the cocatalyst and rhodium trichloride as the catalyst under the conditions of the temperature of 150 ℃ and the pressure of 34 Mpa. Because the high-pressure method has complex separation process, high investment and large energy consumption, the low-pressure method replaces the high-pressure method at present, and the low-pressure methanol carbonylation method is the best production method in the current industrialized method.
The process for synthesizing acetic acid by methanol low-pressure carbonylation mainly comprises two parts, wherein the process for preparing carbon monoxide gas and producing acetic acid is mainly divided into two parts, the gas preparation working section comprises the working procedures of gas preparation, pre-vulcanization, compression molding, desulfurization and decarburization, the production of acetic acid can be divided into a reaction working procedure and a refining working procedure, the reaction working procedure mainly comprises the working procedures of pretreatment, synthesis, conversion and the like, the refining working procedure mainly comprises the working procedures of evaporation, lightness removal, dehydration, distillation, dealkylation, finished product and the like, and the raw materials of the carbon monoxide and the methanol in the gas preparation working section need to be sprayed into a catalytic liquid at high temperature and high pressure (the temperature is 185 ℃ and the pressure is 2..
Based on the process principle of synthesizing acetic acid by methanol low-pressure carbonylation, the existing system and process for synthesizing acetic acid by methanol low-pressure carbonylation have the following problems:
firstly, in the existing system and process for synthesizing acetic acid by methanol low-pressure carbonylation, in the process of preparing acetic acid by introducing methanol and carbon monoxide into catalytic liquid, the gas and the liquid are mixed to generate larger bubbles, and the gas and the liquid cannot be fully mixed due to the larger and larger bubbles, namely, raw materials cannot be fully contacted with the catalytic liquid, so that the reaction rate of the system is reduced, and the acetic acid preparation efficiency is low,
secondly, the energy consumption of the reaction system is complicated due to high temperature, high pressure and stirring conditions.
SUMMERY OF THE UTILITY MODEL
Therefore, the utility model provides a methanol carbonylation with aldehyde is retrieved strengthens reaction system for improve the efficiency of preparing acetic acid among the prior art.
The utility model provides a reaction system is reinforceed in methyl alcohol carbonylation with aldehyde is retrieved, include:
the reactor is used for providing a reaction site for the reaction of the methanol and the carbon monoxide to prepare the required acetic acid;
the number of the micro-interface generators is 2, the micro-interface generators are arranged in the reactors, the two micro-interface generators respectively convert the pressure energy of gas and/or the kinetic energy of liquid into bubble surface energy and transmit the bubble surface energy to gaseous methanol gas and carbon monoxide gas, the methanol gas and the carbon monoxide gas are crushed into micron-sized bubbles with the diameter being more than or equal to 1 mu m and less than 1mm so as to improve the mass transfer area between the catalytic liquid and the methanol gas and the carbon monoxide gas, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the catalytic liquid, the methanol gas and the carbon monoxide gas are mixed into a gas-liquid mixture after being crushed so as to enhance the mass transfer efficiency and the reaction efficiency between the catalytic liquid and the methanol gas and the carbon monoxide gas within a preset operating condition range;
a separation unit disposed at one side of the reactor to separate a product;
a refining unit provided at one side of the reactor to separate a product and produce acetic acid;
and an aldehyde recovery unit disposed at one side of the separation unit to recover the product polyaldehyde.
Further, the micro-interface generator is a pneumatic micro-interface generator, and the micro-interface generator is arranged in the reactor and used for crushing the methanol gas and the carbon monoxide gas to form micron-sized bubbles, outputting the micron-sized bubbles into the reactor after the crushing is finished, and mixing the micron-sized bubbles with the catalytic liquid in the reactor to form a gas-liquid mixture.
Furthermore, a catalytic liquid transmission pipe is communicated with and arranged on the side wall of the upper part of the reactor, a methanol transmission pipe and a carbon monoxide transmission pipe are communicated with and arranged at the lower end of the reactor, and the catalytic liquid transmission pipe, the methanol transmission pipe and the carbon monoxide transmission pipe are respectively used for transmitting catalytic liquid, methanol and carbon monoxide into the reactor.
Further, the separation unit includes:
the flash tank is positioned at one side of the reactor, is communicated with the reactor and is used for carrying out flash separation on a product after the reaction in the reactor is finished;
a first cooler located at the upper side of the reactor and communicating with the reactor for condensing the gas discharged from the top of the reactor.
Further, the refining unit includes:
a light component column, which is communicated with the reactor and the separation unit and is used for removing light components in the resultant;
a dehydration column, wherein the light component column is communicated with the reactor and is used for removing water in the resultant;
a heavy component tower which is communicated with the dehydrating tower and the reactor and is used for removing heavy components in the resultant;
a spent acid stripper in communication with the heavies column and the reactor for stripping spent acid from the product.
Further, the aldehyde recovery unit includes:
a stripping column in communication with the refining unit for stripping polyaldehydes from the product;
a second cooler in communication with the stripping column to cool the polyaldehyde and steam;
a stripping condensate tank communicated with the second cooler and used for collecting condensate in the second cooler;
the polyaldehyde rectifying tower is communicated with the stripping condensate tank and is used for purifying polyaldehyde;
a polyaldehyde intermediate tank communicating with the polyaldehyde rectification column for temporarily storing polyaldehyde; and the polybasic aldehyde recovery tank is communicated with the polybasic aldehyde intermediate tank and is used for storing the recovered polybasic aldehyde.
Further, the polyaldehyde rectifying tower comprises:
a rectifying section located at an upper portion of the polyaldehyde rectifying column to purify the polyaldehyde vapor of the rectifying section;
and the stripping section is positioned at the lower part of the polyaldehyde rectifying tower and is used for increasing the residence time of the condensate in the stripping section, the condensate is in reverse contact with steam at the bottom of the stripping section, the mass transfer and the heat transfer are completed, and the polyaldehyde and impurities are separated plate by plate, so that the acetaldehyde vapor is enriched at the top of the rectifying section.
Further, a stripping medium of the stripping section is steam.
Furthermore, the rectifying section is composed of a plurality of packing layers.
Further, the stripping section consists of a plurality of layers of tower plates.
Compared with the prior art, the beneficial effects of the utility model reside in that, the utility model discloses a broken methyl alcohol gas and carbon monoxide gas make it form micron order bubble of micron yardstick, micron order bubble possesses the physicochemical property that conventional bubble did not possess, can know by the computational formula of spheroid volume and surface area, under the unchangeable circumstances of total volume, the total surface area and the single bubble diameter of bubble are the inverse ratio, can know from this that micron order bubble's total surface area is huge, make micron order bubble and catalytic liquid mix and form gas-liquid mixture, with the area of contact of increase gas-liquid double-phase, and reach the effect of strengthening the mass transfer in lower preset operating condition scope, effectively improve conversion and the efficiency of preparing acetic acid;
furthermore, the micro-interface generator is a pneumatic micro-interface generator, is arranged in the reactor and is used for crushing the methanol gas and the carbon monoxide gas to form micron-sized bubbles, outputting the micron-sized bubbles into the reactor after the crushing is finished and mixing the micron-sized bubbles with the catalytic liquid in the reactor to form a gas-liquid mixture, and effectively improves the conversion rate and efficiency of preparing the acetic acid;
further, a catalyst liquid delivery pipe is communicated with and arranged on the side wall of the upper portion of the reactor, a methanol delivery pipe and a carbon monoxide delivery pipe are communicated with and arranged at the lower end of the reactor, the catalyst liquid delivery pipe, the methanol delivery pipe and the carbon monoxide delivery pipe are respectively used for delivering catalyst liquid, methanol and carbon monoxide into the reactor, the catalyst liquid is delivered into the reactor through the catalyst liquid delivery pipe, then methanol and carbon monoxide are respectively delivered into the two micro-interface generators through the methanol delivery pipe and the carbon monoxide delivery pipe, the temperature of the methanol and the carbon monoxide is 70-80 ℃, the pressure of the methanol and the carbon monoxide is 1.2-1.5MPa, the micro-interface generators crush the methanol gas and the carbon monoxide gas to form micron-scale bubbles, and output the micron-scale bubbles into the reactor after the crushing is finished to be mixed with the catalyst liquid in the reactor to form a gas-liquid mixture, the methanol and the carbon monoxide react under the action of the catalytic liquid to generate byproducts such as acetic acid, polyaldehyde and the like, so that the preparation efficiency of the acetic acid is effectively improved.
Further, the separation unit includes:
the flash tank is positioned at one side of the reactor, is communicated with the reactor and is used for carrying out flash separation on a product after the reaction in the reactor is finished;
the first cooler is positioned on the upper side of the reactor, communicated with the reactor and used for condensing gas discharged from the top of the reactor, products in the reactor enter the flash tank from the reactor, acetic acid, water, methyl iodide, hydrogen iodide polyaldehyde and the like enter the refining unit from the top of the flash tank after flash evaporation, part of catalytic liquid flows back into the reactor from the bottom of the flash tank to continuously participate in the reaction, gas carbon dioxide, hydrogen and methyl iodide in byproducts enter the first cooler from the top of the reactor to be cooled, condensable liquid flows back into the reactor, non-condensable gas is discharged to an external absorption process, and the separation unit is used for primarily separating the products.
Further, the refining unit includes:
a light component column, which is communicated with the reactor and the separation unit and is used for removing light components in the resultant;
a dehydration column, wherein the light component column is communicated with the reactor and is used for removing water in the resultant;
a heavy component tower which is communicated with the dehydrating tower and the reactor and is used for removing heavy components in the resultant;
the waste acid stripping tower is communicated with the heavy component tower and the reactor and is used for stripping waste acid in a product, a mixture entering the refining unit is firstly condensed in the light component tower, condensed liquid methyl iodide and hydrogen iodide return to the reactor, acetic acid, water and multi-element aldehyde enter the dehydrating tower from the light component tower, the product acetic acid in the dehydrating tower enters the heavy component tower after being dehydrated, the heavy component tower removes by-product heavy hydrocarbon substances in the acetic acid and then enters the waste acid stripping tower, the waste acid stripping tower separates by-product propionic acid in the acetic acid and produces the product acetic acid, and the refining unit further removes impurities from the product to produce purer acetic acid.
Further, the aldehyde recovery unit includes:
a stripping column in communication with the refining unit for stripping polyaldehydes from the product;
a second cooler in communication with the stripping column to cool the polyaldehyde and steam;
a stripping condensate tank communicated with the second cooler and used for collecting condensate in the second cooler;
the polyaldehyde rectifying tower is communicated with the stripping condensate tank and is used for purifying polyaldehyde;
a polyaldehyde intermediate tank communicating with the polyaldehyde rectification column for temporarily storing polyaldehyde;
the multi-aldehyde recovery tank is communicated with the multi-aldehyde intermediate tank and used for storing recovered multi-aldehyde, the multi-aldehyde enters the aldehyde recovery unit from the waste acid stripping tower, firstly, the multi-aldehyde is stripped in the stripping tower by adopting a steam stripping process to form mixed gas of the multi-aldehyde and water vapor, the mixed gas of the multi-aldehyde and the water vapor enters the second cooler, condensate enters the stripping condensate tank through the second cooler, and the multi-aldehyde recovery unit effectively recovers byproduct multi-aldehyde.
Further, the polyaldehyde rectifying tower comprises:
a rectifying section located at an upper portion of the polyaldehyde rectifying column to purify the polyaldehyde vapor of the rectifying section;
and the stripping section is positioned at the lower part of the polyaldehyde rectifying tower and is used for increasing the residence time of the condensate in the stripping section, the condensate is in reverse contact with steam at the bottom of the stripping section, the mass transfer and the heat transfer are completed, and the polyaldehyde and impurities are separated plate by plate, so that the acetaldehyde vapor is enriched at the top of the rectifying section.
Furthermore, the rectifying section is composed of a plurality of packing layers.
Furthermore, the stripping section is composed of a plurality of layers of tower plates, condensate in the stripping condensate tank enters the multi-aldehyde rectifying tower, the condensate continuously flows downwards in the stripping section under the action of gravity, the stripping section is composed of a plurality of layers of tower plates, the residence time of the condensate in the stripping section is prolonged, the condensate reversely contacts steam at the bottom of the stripping section to complete mass transfer and heat transfer, and multi-aldehyde and impurities are separated plate by plate, so that acetaldehyde vapor is enriched at the top of the rectifying section and then discharged into the multi-aldehyde intermediate tank, samples in the multi-aldehyde intermediate tank are sampled, and after the samples are qualified, all the multi-aldehyde is discharged into the multi-aldehyde recovery tank, so that the recovered multi-aldehyde is relatively pure.
Drawings
FIG. 1 is a schematic diagram of a methanol carbonylation-enhanced reaction system with aldehyde recovery according to the present invention.
Detailed Description
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 diagram of a methanol carbonylation enhanced reaction system with aldehyde recovery according to the present invention is shown, which includes:
the reactor 1 is used for providing a reaction site for the reaction of methanol and carbon monoxide to prepare the required acetic acid;
the micro-interface generators 2 are arranged in the reactors, the two micro-interface generators respectively convert the pressure energy of gas and/or the kinetic energy of liquid into bubble surface energy and transmit the bubble surface energy to gaseous methanol gas and carbon monoxide gas, the methanol gas and the carbon monoxide gas are crushed into micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm so as to improve the mass transfer area between the catalytic liquid and the methanol gas and the carbon monoxide gas, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the catalytic liquid, the methanol gas and the carbon monoxide gas are mixed into a gas-liquid mixture after being crushed so as to enhance the mass transfer efficiency and the reaction efficiency between the catalytic liquid and the methanol gas and the carbon monoxide gas within a preset micron-sized operating condition range;
a separation unit 3 provided at one side of the reactor to separate a product;
a purification unit 4 provided at one side of the reactor, for separating a product to produce acetic acid;
and an aldehyde recovery unit 5 provided at one side of the separation unit to recover the product polyaldehyde.
With reference to fig. 1, the micro-interface generator is a pneumatic micro-interface generator, and the micro-interface generator is disposed in the reactor and is configured to crush the methanol gas and the carbon monoxide gas to form micron-sized bubbles, and output the micron-sized bubbles into the reactor after the crushing is completed to mix with the catalytic liquid in the reactor to form a gas-liquid mixture, so as to effectively improve the conversion rate and efficiency of preparing acetic acid;
continuing to refer to fig. 1, a catalyst liquid delivery tube 101 is communicated with and disposed on an upper side wall of the reactor, a methanol delivery tube 102 and a carbon monoxide delivery tube 103 are communicated with and disposed at a lower end of the reactor, the catalyst liquid delivery tube, the methanol delivery tube and the carbon monoxide delivery tube are respectively used for delivering catalyst liquid, methanol and carbon monoxide into the reactor, the catalyst liquid is delivered into the reactor through the catalyst liquid delivery tube, then methanol and carbon monoxide are respectively delivered into the two micro interface generators through the methanol delivery tube and the carbon monoxide delivery tube, the temperature of methanol and carbon monoxide is 70-80 ℃, the pressure is 1.2-1.5Mpa, the micro interface generators crush methanol gas and carbon monoxide gas to form micron-sized bubbles, and the micron-sized bubbles are output into the reactor and mixed with the catalyst liquid in the reactor to form a gas-liquid mixture after the crushing is completed, the methanol and the carbon monoxide react under the action of the catalytic liquid to generate byproducts such as acetic acid, polyaldehyde and the like, so that the preparation efficiency of the acetic acid is effectively improved.
With continued reference to fig. 1, the separation unit includes:
a flash tank 301, which is located at one side of the reactor, is communicated with the reactor, and is used for performing flash separation on a product after the reaction in the reactor is completed;
the first cooler 302 is located on the upper side of the reactor, is communicated with the reactor, and is used for condensing gas discharged from the top of the reactor, the product in the reactor enters the flash tank from the reactor, acetic acid, water, methyl iodide, hydrogen iodide polyaldehyde and the like enter the refining unit from the top of the flash tank after flash evaporation, meanwhile, part of the catalytic liquid flows back into the reactor from the bottom of the flash tank to continue to participate in the reaction, gas carbon dioxide, hydrogen and methyl iodide in byproducts enter the first cooler from the top of the reactor to be cooled, condensable liquid flows back into the reactor, non-condensable gas is discharged to an external absorption process, and the separation unit is used for primarily separating the product.
With continued reference to fig. 1, the refining unit includes:
a light component column 401, communicating with the reactor and the separation unit, for removing light components from the resultant;
a dehydration column 402, in communication with the reactor, for removing water from the product;
a heavy component tower 403 which is communicated with the dehydration tower and the reactor and is used for removing heavy components in the resultant;
and a waste acid stripping tower 404, which is communicated with the heavy component tower and the reactor, and is used for stripping waste acid in a product, wherein a mixture entering the refining unit is firstly condensed in the light component tower, condensed liquid methyl iodide and hydrogen iodide return to the reactor, acetic acid, water and multi-aldehyde enter the dehydrating tower from the light component tower, the product acetic acid in the dehydrating tower is dehydrated and enters the heavy component tower, the heavy component tower removes by-product heavy hydrocarbon substances in the acetic acid and then enters the waste acid stripping tower, the by-product propionic acid in the acetic acid is separated by the stripping tower and is discharged as the product acetic acid, and the refining unit further removes impurities from the product to generate purer waste acid.
With continued reference to fig. 1, the aldehyde recovery unit includes:
a stripping column 501, which is communicated with the refining unit and is used for stripping the polyaldehyde in the product;
a second cooler 502 in communication with the stripping column to cool the polyaldehyde and steam;
a stripping condensate tank 503, which is communicated with the second cooler and is used for collecting condensate in the second cooler;
a polyaldehyde rectification column 504, which is communicated with the stripping condensate tank and is used for purifying polyaldehyde;
a polyaldehyde intermediate tank 505 communicating with the polyaldehyde rectification column for temporarily storing the polyaldehyde;
the multi-aldehyde recovery tank 506 is communicated with the multi-aldehyde intermediate tank and used for storing recovered multi-aldehyde, the multi-aldehyde enters the aldehyde recovery unit from the waste acid stripping tower, firstly, the multi-aldehyde is stripped in the stripping tower by adopting a steam stripping process to form mixed gas of the multi-aldehyde and water vapor, the mixed gas of the multi-aldehyde and the water vapor enters the second cooler, condensate enters the stripping condensate tank through the second cooler, and the multi-aldehyde recovery unit effectively recovers byproduct multi-aldehyde.
With continuing reference to fig. 1, the polyaldehyde rectification column comprises:
a rectifying section 5041 located at an upper portion of the polyaldehyde rectifying column to purify the polyaldehyde vapor of the rectifying section;
a stripping section 5042 which is positioned at the lower part of the polyaldehyde rectifying tower and is used for increasing the residence time of condensate in the stripping section, the condensate is in reverse contact with steam at the bottom of the stripping section, the mass transfer and the heat transfer are completed, and the polyaldehyde is separated from impurities plate by plate, so that the acetaldehyde vapor is enriched at the top of the rectifying section.
The rectifying section is composed of a plurality of packing layers.
The stripping section consists of a plurality of layers of tower plates, condensate in the stripping condensate tank enters the multi-aldehyde rectifying tower, condensate continuously flows downwards in the stripping section under the action of gravity, the stripping section consists of a plurality of layers of tower plates, the residence time of the condensate in the stripping section is prolonged, the condensate reversely contacts steam at the bottom of the stripping section to complete mass transfer and heat transfer, and multi-aldehyde and impurities are separated plate by plate, so that acetaldehyde steam is enriched at the top of the rectifying section and then discharged into the multi-aldehyde intermediate tank, samples in the multi-aldehyde intermediate tank are sampled, and after the samples are qualified, all the multi-aldehyde is discharged into the multi-aldehyde recovery tank, so that the recovered multi-aldehyde is relatively pure.
With continued reference to fig. 1, the present invention provides a methanol carbonylation enhanced reaction system with aldehyde recovery, comprising:
step 1: firstly, the catalyst liquid is transmitted into the reactor through the catalyst liquid transmission pipe, then methanol and carbon monoxide are respectively transmitted into the two micro-interface generators through the methanol transmission pipe and the carbon monoxide transmission pipe, the temperature of the methanol and the carbon monoxide is 70-80 ℃, the pressure of the methanol and the carbon monoxide is 1.2-1.5Mpa, the micro-interface generators crush the methanol gas and the carbon monoxide gas to form micron-scale micron-sized bubbles, the micron-sized bubbles are output into the reactor after the crushing is finished and are mixed with the catalyst liquid in the reactor to form a gas-liquid mixture, and the methanol and the carbon monoxide react under the action of the catalyst liquid to generate byproducts such as acetic acid, multi-aldehyde and the like;
step 2: the product in the reactor in the step 1 enters the flash tank from the reactor, acetic acid, water, methyl iodide, hydrogen iodide polyaldehyde and the like enter the refining unit from the top of the flash tank after flash evaporation, meanwhile, part of catalytic liquid flows back to the reactor from the bottom of the flash tank to continuously participate in reaction, gas carbon dioxide, hydrogen and methyl iodide in byproducts enter the first cooler from the top of the reactor to be cooled, condensable liquid flows back to the reactor, and non-condensable gas is discharged to an external absorption process;
and step 3: the mixture entering the refining unit in the step 2 is condensed in the light component tower, wherein condensate methyl iodide and hydrogen iodide return to the reactor, acetic acid, water and polyaldehyde enter the dehydrating tower from the light component tower, the product acetic acid in the dehydrating tower is dehydrated and enters the heavy component tower, the heavy component tower removes heavy hydrocarbon substances of the by-product in the acetic acid and then enters the waste acid stripping tower, and the waste acid stripping tower separates the by-product propionic acid in the acetic acid and produces the product acetic acid;
and 4, step 4: the polybasic aldehyde enters the aldehyde recovery unit from the waste acid stripping tower, firstly, the polybasic aldehyde is stripped in the stripping tower by adopting a steam stripping process to form mixed gas of the polybasic aldehyde and water vapor, the mixed gas of the polybasic aldehyde and the water vapor enters the second cooler, and condensate liquid of the polybasic aldehyde and the water vapor enters the stripping condensate liquid tank through the second cooler;
and 5: and 4, feeding the condensate in the steam stripping condensate tank into the polyaldehyde rectifying tower, enabling the condensate to continuously flow downwards in a stripping section under the action of gravity, enabling the stripping section to consist of multiple layers of tower plates, increasing the residence time of the condensate in the stripping section, enabling the condensate to be in reverse contact with steam at the bottom of the stripping section to finish mass transfer and heat transfer, separating polyaldehyde from impurities plate by plate, enabling acetaldehyde vapor to be enriched at the top of the rectifying section, then discharging the acetaldehyde vapor into the polyaldehyde intermediate tank, sampling samples in the polyaldehyde intermediate tank, and discharging all the polyaldehyde into the polyaldehyde recovery tank after the polyaldehyde is qualified.
Example 1
The acetic acid is prepared by using the system and the process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 75 ℃, the inlet air pressure is 1.1Mpa, the temperature in the reactor is 85 ℃, the pressure is 1.1Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The gas-liquid ratio in the micro-interface generator is 600: 1.
through detection, after the system and the process are used, the purity of the prepared acetic acid is 99.8%, and the preparation time is 12 hours.
Example 2
The acetic acid is prepared by using the system and the process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 75 ℃, the inlet air pressure is 1.1Mpa, the temperature in the reactor is 85 ℃, the pressure is 1.1Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The gas-liquid ratio in the micro-interface generator is 600: 1.
through detection, after the system and the process are used, the purity of the prepared acetic acid is 99.8%, and the preparation time is 11.5 h.
Example 3
The acetic acid is prepared by using the system and the process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 75 ℃, the inlet air pressure is 1.1Mpa, the temperature in the reactor is 85 ℃, the pressure is 1.1Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The gas-liquid ratio in the micro-interface generator is 600: 1.
through detection, after the system and the process are used, the purity of the prepared acetic acid is 99.8%, and the preparation time is 12 hours.
Example 4
The acetic acid is prepared by using the system and the process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 75 ℃, the inlet air pressure is 1.1Mpa, the temperature in the reactor is 85 ℃, the pressure is 1.1Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The gas-liquid ratio in the micro-interface generator is 600: 1.
through detection, after the system and the process are used, the purity of the prepared acetic acid is 99.8%, and the preparation time is 12 hours.
Example 5
The acetic acid is prepared by using the system and the process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 75 ℃, the inlet air pressure is 1.1Mpa, the temperature in the reactor is 85 ℃, the pressure is 1.1Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The gas-liquid ratio in the micro-interface generator is 600: 1.
through detection, after the system and the process are used, the purity of the prepared acetic acid is 99.8%, and the preparation time is 12 hours.
Example 6
The acetic acid is prepared by using the system and the process, wherein:
the inlet air temperature of the methanol and the carbon monoxide is 75 ℃, the inlet air pressure is 1.1Mpa, the temperature in the reactor is 85 ℃, the pressure is 1.1Mpa, and the ratio of the inlet air quantity of the methanol and the carbon monoxide is 1: 1.
The gas-liquid ratio in the micro-interface generator is 600: 1.
through detection, after the system and the process are used, the purity of the prepared acetic acid is 99.8%, and the preparation time is 12 hours.
Comparative example
Acetic acid production was carried out using a prior art methanol carbonylation process, wherein the process parameters selected for this comparative example were the same as those described in example 6.
The detection proves that the purity of the prepared acetic acid is 89%, and the preparation time is 33 h.
So far, the technical solution of the present invention has been described with reference to the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, a person skilled in the art can make equivalent changes or substitutions to the related technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A methanol carbonylation-enhanced reaction system with aldehyde recovery, comprising:
the reactor is used for providing a reaction site for the reaction of the methanol and the carbon monoxide to prepare the required acetic acid;
the number of the micro-interface generators is 2, the micro-interface generators are arranged in the reactors, the two micro-interface generators respectively convert the pressure energy of gas and/or the kinetic energy of liquid into bubble surface energy and transmit the bubble surface energy to gaseous methanol gas and carbon monoxide gas, the methanol gas and the carbon monoxide gas are crushed into micron-sized bubbles with the diameter being more than or equal to 1 mu m and less than 1mm so as to improve the mass transfer area between the catalytic liquid and the methanol gas and the carbon monoxide gas, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the catalytic liquid, the methanol gas and the carbon monoxide gas are mixed into a gas-liquid mixture after being crushed so as to enhance the mass transfer efficiency and the reaction efficiency between the catalytic liquid and the methanol gas and the carbon monoxide gas within a preset operating condition range;
a separation unit disposed at one side of the reactor;
a refining unit disposed at one side of the reactor;
an aldehyde recovery unit disposed at one side of the separation unit.
2. The system of claim 1, wherein the micro-interface generator is a pneumatic micro-interface generator, and the micro-interface generator is disposed in the reactor to crush the methanol gas and the carbon monoxide gas into micron-sized bubbles and output the micron-sized bubbles into the reactor after the crushing is completed and mix the micron-sized bubbles with the catalyst solution in the reactor to form a gas-liquid mixture.
3. The system of claim 1, wherein a catalyst liquid delivery pipe is connected to the upper side wall of the reactor, and a methanol delivery pipe and a carbon monoxide delivery pipe are connected to the lower end of the reactor, and the catalyst liquid delivery pipe, the methanol delivery pipe and the carbon monoxide delivery pipe are used for delivering catalyst liquid, methanol and carbon monoxide into the reactor respectively.
4. The methanol carbonylation-enhanced reaction system with aldehyde recovery of claim 1, wherein the separation unit comprises:
the flash tank is positioned at one side of the reactor, is communicated with the reactor and is used for carrying out flash separation on a product after the reaction in the reactor is finished;
a first cooler located at the upper side of the reactor and communicating with the reactor for condensing the gas discharged from the top of the reactor.
5. The system of claim 1, wherein the refining unit comprises:
a light component column, which is communicated with the reactor and the separation unit and is used for removing light components in the resultant;
a dehydration column, wherein the light component column is communicated with the reactor and is used for removing water in the resultant;
a heavy component tower which is communicated with the dehydrating tower and the reactor and is used for removing heavy components in the resultant;
a spent acid stripper in communication with the heavies column and the reactor for stripping spent acid from the product.
6. The methanol carbonylation-enhanced reaction system with aldehyde recovery of claim 1, wherein the aldehyde recovery unit comprises:
a stripping column in communication with the refining unit for stripping polyaldehydes from the product;
a second cooler in communication with the stripping column to cool the polyaldehyde and steam;
a stripping condensate tank communicated with the second cooler and used for collecting condensate in the second cooler;
the polyaldehyde rectifying tower is communicated with the stripping condensate tank and is used for purifying polyaldehyde;
a polyaldehyde intermediate tank communicating with the polyaldehyde rectification column for temporarily storing polyaldehyde;
and the polybasic aldehyde recovery tank is communicated with the polybasic aldehyde intermediate tank and is used for storing the recovered polybasic aldehyde.
7. The methanol carbonylation with aldehyde recovery enhanced reaction system of claim 6, wherein the polyaldehyde rectification column comprises:
a rectifying section located at an upper portion of the polyaldehyde rectifying column to purify the polyaldehyde vapor of the rectifying section;
and the stripping section is positioned at the lower part of the polyaldehyde rectifying tower and is used for increasing the residence time of the condensate in the stripping section, the condensate is in reverse contact with steam at the bottom of the stripping section to complete mass transfer and heat transfer, and polyaldehyde and impurities are separated plate by plate, so that acetaldehyde vapor is enriched at the top of the rectifying section.
8. The system of claim 7, wherein the stripping medium of the stripping section is steam.
9. The system of claim 7, wherein the rectifying section comprises a plurality of packing layers.
10. The system of claim 7, wherein the stripping section comprises a plurality of stages.
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