CN114644550B - Reaction system and process for preparing acetic acid by methanol carbonylation - Google Patents
Reaction system and process for preparing acetic acid by methanol carbonylation Download PDFInfo
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- CN114644550B CN114644550B CN202011520544.2A CN202011520544A CN114644550B CN 114644550 B CN114644550 B CN 114644550B CN 202011520544 A CN202011520544 A CN 202011520544A CN 114644550 B CN114644550 B CN 114644550B
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 171
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 91
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 33
- 230000006315 carbonylation Effects 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 13
- 239000000376 reactant Substances 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 19
- 239000012263 liquid product Substances 0.000 claims description 18
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 17
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 230000009471 action Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 230000003014 reinforcing effect Effects 0.000 claims description 5
- 229920001744 Polyaldehyde Polymers 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000003973 paint Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 29
- 238000001514 detection method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 3
- 238000005728 strengthening Methods 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
- 150000001299 aldehydes Chemical class 0.000 description 2
- 239000013064 chemical raw material Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000008859 change Effects 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
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
Abstract
The invention relates to a reaction system and a process for preparing acetic acid by methanol carbonylation, wherein the reaction system comprises the following steps: reaction vessel, vessel shell, vessel liner, etc. The reaction container is arranged to be in a structure that the container shell and the container liner are combined, the reaction container comprises a container shell, a container liner and a container sealing cover, the container liner is positioned in the container shell, the inner wall of the container liner is used for replacing the container shell to be in contact with reactants, the container sealing cover is used for sealing the open end of the reaction container, the side wall of the container liner is coated with anti-corrosion paint, the container liner can be used for replacing the container shell to be in contact with the reactants, and therefore the purpose that the whole reaction container is not required to be replaced can be achieved only by regularly replacing the container liner, and the equipment cost is effectively reduced.
Description
Technical Field
The invention relates to the technical field of acetic acid preparation, in particular to a reaction system and a process for preparing acetic acid by methanol carbonylation.
Background
Acetic acid is an important basic organic chemical raw material, and is synthesized from main raw materials such as chloroacetic acid, vinyl acetate monomer, polyvinyl alcohol, terephthalic acid, acetate fiber, metal acetate and the like, and has wide application in various aspects such as pesticides, medicines, dyes, adhesives, organic solvents and the like along with scientific development.
As an important chemical raw material with wide application, the synthesis method of acetic acid mainly includes fermentation of carbohydrate, oxidation of naphtha or n-butane, oxidation of ethylene or acetaldehyde, carbonylation of methanol and the like, wherein the methanol carbonylation method accounts for 60% of the current world acetic acid production, methanol and carbon monoxide are used as raw materials for synthesizing the acetic acid through carbonylation, the method has the main advantages of fewer byproducts, diversified raw material routes and coal char, natural gas and heavy oil as basic raw materials, and is particularly suitable for coal chemical industry, and has the advantages of less three wastes, long service life, less consumption, high catalyst activity and easy treatment. The low pressure process in methanol carbonylation is to use rhodium as main catalyst and iodide as cocatalyst to synthesize acetic acid at 150-200 deg.c and 3-6MPa pressure, and to avoid rhodium catalyst deposition and raise reaction rate, water is added into the system.
The methanol carbonylation process has inherent defects that the existence of the iodide as a promoter can cause serious corrosion to equipment, so that the equipment is frequently replaced as a whole, the investment cost is high, and the product separation is difficult due to a large amount of water existing in the system, so that the purity of the product is low.
Disclosure of Invention
Therefore, the invention provides a reaction system and a process for preparing acetic acid by methanol carbonylation, which are used for solving the problems that the existence of cocatalyst iodide can cause serious corrosion to equipment in the prior art, and meanwhile, a large amount of water existing in the system for preparing acetic acid by the methanol carbonylation method causes difficult separation of products and low purity of the products.
The invention provides a reaction system for preparing acetic acid by methanol carbonylation, which comprises the following steps:
the reaction container is used for providing a reaction place for the carbonylation reaction of the methanol and comprises a container shell, a container liner and a container closing cover, wherein the container liner is positioned in the container shell, the inner wall of the container liner replaces the container shell to be contacted with reactants, and the container closing cover is used for closing the opening end of the reaction container;
the bottom wall of the container liner is in a convex shape along the vertical upward direction, a reserved cavity is formed between the bottom wall of the container liner and the bottom wall of the container shell, and a fixing component for fixing the container liner is arranged in the reserved cavity;
a flash tank which is communicated with the reaction vessel and is used for carrying out flash separation on the products in the reaction vessel;
a cooler in communication with the reaction vessel and the flash tank for condensing the gas exiting the top of the reaction vessel and the gas exiting the flash tank;
and the evaporator is communicated with the flash tank and the cooler and is used for purifying the liquid product discharged from the flash tank and the liquid product discharged from the cooler.
Preferably, the fixed subassembly includes the compensation plate, the both sides wall of symmetry on the compensation plate is cambered surface lateral wall and plane lateral wall respectively, the cambered surface lateral wall of compensation plate with the diapire fixed connection of container inner bag, on the plane lateral wall of compensation plate with all fixedly connected with first spread groove and the second spread groove that mutually support the use on the diapire in the container shell, the one end of fixed connection spring in the second spread groove, the other end of spring with first spread groove joint.
Preferably, the lower end of the container closing cover is fixedly connected with an annular clamping groove for fixing the container liner.
Preferably, an annular compensation strip equal to the difference in height between the container liner and the container shell is arranged in the annular clamping groove.
Preferably, a locking component for fixing the container closing cover is arranged on the side wall of the annular clamping groove.
Preferably, the lock catch assembly comprises symmetrically arranged connecting blocks, lock plates are connected to the connecting blocks in a rotating mode, lock holes are formed in the lock plates and the side walls of the reaction container, and lock bolts penetrate through the lock plates.
Preferably, the inside of the container closing cover is of a cavity structure, and reinforcing ribs are arranged in the container closing cover.
Preferably, the material conveying pipe and the gas discharging pipe are arranged on the container closing cover.
Preferably, the main part of the evaporator is a square tank, a spoiler group is uniformly arranged in the evaporator, the spoiler group consists of two inclined panels arranged in the vertical direction, the inclined panels are square panels, one ends of the inclined panels are fixedly connected with the inner side walls of the evaporator, and the free ends of the inclined panels are positioned on the upper sides of the fixed ends.
The invention provides a reaction process for preparing acetic acid by methanol carbonylation, which comprises the following steps:
step 1: the catalyst solution is conveyed into the reaction vessel through a material conveying pipe arranged on the vessel sealing cover, gaseous carbon monoxide and gaseous methanol are conveyed into the reaction vessel through a material conveying pipe arranged on the vessel sealing cover, the carbon monoxide and the gaseous methanol are subjected to methanol carbonylation reaction under the action of a catalyst to synthesize acetic acid and polyaldehyde, and the vessel liner in the reaction vessel is replaced periodically;
step 2: the liquid product in the reaction vessel enters the flash tank under the action of pump force, the gas in the reaction vessel is discharged into the cooler along the top, after the liquid product in the flash tank is flashed, a gas phase part comprises a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde, the gas phase part is discharged into the cooler from the top of the flash tank, the liquid phase part enters the evaporator for purifying acetic acid, after the gas in the cooler is cooled, the condensable liquid flows into the evaporator, the non-condensable gas is discharged to an external absorption process, and the flash tank and the cooler finish primary separation of the product;
step 3: the liquid phase part from the flash tank and the cooler enters from the upper part of the evaporator, a flow blocking plate group uniformly arranged in the liquid phase part along the inside of the evaporator flows from top to bottom, the temperature control in the inside of the evaporator is controlled at 100-105 ℃, water and multi-aldehyde part in the liquid phase part are gradually evaporated to be gas phase and discharged into an external collecting tank along the top of the evaporator, and the rest liquid phase part is acetic acid and discharged along the bottom of the evaporator.
Compared with the prior art, the invention has the beneficial effects that the reaction container is provided with the structure of combining the container shell and the container liner, the reaction container comprises the container shell, the container liner and the container sealing cover, the container liner is positioned in the container shell, the inner wall of the container liner replaces the container shell to be contacted with reactants, the container sealing cover is used for sealing the open end of the reaction container, the side wall of the container liner is coated with the anti-corrosion coating, and the container liner can replace the container shell to be contacted with the reactants, so that the integral purpose of the reaction container can be achieved without replacing the container liner only by periodically replacing the container liner, thereby effectively reducing the equipment cost;
the bottom wall of the container liner is in a convex shape along the vertical upward direction, a reserved cavity is formed between the bottom wall of the container liner and the bottom wall of the container shell, a fixing component for fixing the container liner is arranged in the reserved cavity, and the reserved cavity is used for providing an installation space for the fixing component, so that the container liner is firmly fixed in the container shell by the fixing component, and meanwhile, the purpose of easy replacement is achieved;
the flash tank is communicated with the reaction vessel and used for carrying out flash separation on the products in the reaction vessel, and the liquid products in the reaction vessel enter the flash tank under the action of pump force to carry out gas-liquid flash separation;
the cooler is communicated with the reaction vessel and the flash tank and is used for condensing the gas discharged from the top of the reaction vessel and the gas discharged from the flash tank, after the liquid product in the flash tank is subjected to flash evaporation, a gas phase part comprises a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde, the gas in the cooler 7 is discharged into the cooler from the top of the flash tank, after being cooled, the condensable liquid flows to the evaporator, the non-condensable gas is discharged to an external absorption process, and the flash tank and the cooler finish the primary separation of the product;
the evaporator is communicated with the flash tank and the cooler and is used for purifying liquid products discharged from the flash tank and liquid products discharged from the cooler, liquid phase parts of the flash tank and the cooler enter the evaporator to be subjected to acetic acid purification, flow baffle groups are uniformly arranged in the liquid phase parts along the interior of the evaporator from top to bottom, the temperature of the interior of the evaporator is controlled to be 100-105 ℃, water and multi-aldehyde parts in the liquid phase parts are gradually evaporated to be gas phase and discharged into an external collecting tank along the top of the evaporator, and the rest liquid phase parts are acetic acid and are discharged along the bottom of the evaporator.
Further, the fixed subassembly includes the compensation plate, the both sides wall of symmetry is cambered surface lateral wall and plane lateral wall respectively on the compensation plate, cambered surface lateral wall and the diapire fixed connection of container inner bag, all fixedly connected with each other on the plane lateral wall of compensation plate and the container shell inner wall use first spread groove and second spread groove, the one end of fixed connection spring in the second spread groove, the other end and the first spread groove joint of spring, the setting of compensation plate is used for compensating the arc diapire of container inner bag, thereby constitute a flat connection plane, be convenient for the connection of first spread groove, the container inner bag is located the container shell inside, the spring has certain vertically ascending effort to it, make the container inner bag card between container closing cap and fixed subassembly, consequently, container inner bag is in the fixed state in container shell inside under container closing cap keeps the confined state, when container inner bag need be changed, only need be opened the container closing cap, take out the container inner bag, fixed subassembly realizes firmly fixing the container inner bag in the container shell, reach the purpose of easily changing simultaneously.
Further, the lower end fixedly connected with of container closing lid is used for fixed container inner bag's annular draw-in groove, and when container closing lid was the confined state, the upper end of container shell and container inner bag all was located annular draw-in groove, and the annular draw-in groove plays the fixed effect to the upper end of container inner bag from this.
Further, an annular compensation strip which is equal to the difference between the heights of the container liner and the container shell is arranged in the annular clamping groove. The height of the container liner is smaller than that of the container shell, and the annular compensation strips are used for compensating the height difference between the container liner and the container shell and further fixing the upper end of the container liner 3 in an omnibearing manner.
Further, a lock catch assembly used for fixing the container closing cover is arranged on the side wall of the annular clamping groove, and the container closing cover is locked at the opening of the upper end of the reaction container by the aid of the lock catch assembly, so that the reaction container is closed.
Further, the lock catch assembly comprises a symmetrically arranged connecting block, the connecting block is rotationally connected with a lock plate, a lock hole is formed in the lock plate and the side wall of the reaction container, a lock bolt penetrates through the lock plate, the lock plate can rotate under the action of external force, the lock bolt is fixed on the lock plate and the lock hole formed in the side wall of the reaction container, so that the lock plate is fixed, the container closing cover is locked at the upper end opening of the reaction container, and the reaction container is closed.
Further, the inside of container closing lid is cavity structure, and the inside of container closing lid is provided with the strengthening rib, and the inside of container closing lid has alleviateed the weight of container closing lid self to a certain extent for cavity structure, the change of the container inner bag of inside of further being convenient for, and the setting of strengthening rib is used for strengthening the intensity of container closing lid.
Further, the main part of evaporimeter is square jar body, the inside of evaporimeter evenly is provided with the spoiler group, the spoiler group comprises two inclined plane boards that set up in vertical direction, inclined plane board is square panel, inclined plane board's one end and the inside wall fixed connection of evaporimeter, inclined plane board's free end is located the upside of stiff end, liquid phase part evenly is provided with the spoiler group along the inside of evaporimeter from top to bottom and flows, liquid phase part gradually flows along inclined plane board, because inclined plane board's free end is located the upside of stiff end, therefore liquid phase part all need be under the effect of piling up of follow-up fluid through an inclined plane board, the effectual circulation time of liquid phase part in the evaporimeter that has increased ensures that water and many aldehydes part in the liquid phase part are evaporated completely, improve acetic acid purity.
Drawings
FIG. 1 is a schematic diagram of the reaction system for preparing acetic acid by methanol carbonylation according to the present invention;
FIG. 2 is an enlarged schematic view of the invention at A in FIG. 1;
FIG. 3 is an enlarged schematic view of the invention at B in FIG. 1;
fig. 4 is a top cross-sectional view of the evaporator and inclined panel of the present invention.
In the figure: 1-reaction vessel, 2-vessel shell, 3-vessel liner, 4-vessel closing cap, 5-fixing component, 501-compensation plate, 502-first connecting slot, 503-second connecting slot, 504-spring, 6-flash tank, 7-cooler, 8-evaporator, 9-annular clamping slot, 10-annular compensation strip, 11-latch component, 111-connecting block, 112-latch plate, 113-latch, 12-reinforcing rib, 13-inclined panel, 14-reserved cavity.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are merely for explaining the technical principles of the present invention, and are not intended to limit the scope of the present invention.
Referring to fig. 1, which is a schematic structural diagram of a reaction system for preparing acetic acid by carbonylation of methanol according to the present invention, a reaction system for preparing acetic acid by carbonylation of methanol comprises:
the reaction container 1 is used for providing a reaction place for the carbonylation reaction of methanol, the reaction container 1 comprises a container shell 2, a container liner 3 and a container closing cover 4, the container liner 3 is positioned in the container shell 2, the inner wall of the container liner 3 replaces the container shell 2 to be contacted with reactants, the container closing cover 4 is used for closing the open end of the reaction container 1, the side wall of the container liner 3 is coated with anti-corrosion paint, and the container liner 3 can replace the container shell 2 to be contacted with reactants, so that the purpose of not needing to replace the whole reaction container can be achieved only by periodically replacing the container liner 3, and the equipment cost is effectively reduced;
the bottom wall of the container liner 3 is in a convex shape along the vertical upward direction, a reserved cavity 14 is formed between the bottom wall of the container liner 3 and the bottom wall of the container shell 2, a fixing component 5 for fixing the container liner 3 is arranged in the reserved cavity 14, and the reserved cavity 14 is used for providing an installation space for the fixing component 5, so that the fixing component 5 stably fixes the container liner 3 in the container shell 2 and simultaneously achieves the aim of easy replacement;
a flash tank 6 which is communicated with the reaction vessel 1 and is used for carrying out flash evaporation separation on the products in the reaction vessel 1, wherein the liquid products in the reaction vessel 1 enter the flash tank 6 under the action of pump force to carry out gas-liquid flash evaporation separation;
a cooler 7 which is communicated with the reaction vessel 1 and the flash tank 6 and is used for condensing the gas discharged from the top of the reaction vessel 1 and the gas discharged from the flash tank 6, wherein after the liquid product in the flash tank 6 is flashed, a gas phase part comprises a small amount of acetic acid, water, a small amount of catalyst components and multi-component aldehyde, the gas phase part is discharged into the cooler 7 from the top of the flash tank 6, the gas in the cooler 7 is cooled and then the condensable liquid flows to the evaporator 8, the non-condensable gas is discharged to an external absorption process, and the flash tank 6 and the cooler 7 finish the primary separation of the product;
the evaporator 8 is communicated with the flash tank 6 and the cooler 7, and is used for purifying the liquid product discharged from the flash tank 6 and the liquid product discharged from the cooler 7, the flash tank 6 and the liquid phase part of the cooler 7 enter the evaporator 8 to be subjected to acetic acid purification, a flow blocking plate group uniformly arranged in the liquid phase part along the interior of the evaporator 8 flows from top to bottom, the temperature of the interior of the evaporator 8 is controlled to be 100-105 ℃, water and multi-aldehyde part in the liquid phase part are gradually evaporated to form a gas phase, the gas phase is discharged to an external collecting tank along the top of the evaporator 8, and the rest liquid phase part is discharged along the bottom of the evaporator 8.
Referring to fig. 3, specifically, the fixing component 5 includes a compensation plate 501, two symmetrical side walls on the compensation plate 501 are respectively an arc side wall and a plane side wall, the arc side wall of the compensation plate 501 is fixedly connected with the bottom wall of the container liner 3, a first connecting groove 502 and a second connecting groove 503 which are mutually matched and used are fixedly connected on the plane side wall of the compensation plate 501 and the bottom wall of the container liner 2, one end of a spring 504 is fixedly connected in the second connecting groove 503, the other end of the spring 504 is clamped with the first connecting groove 502, the arrangement of the compensation plate 501 is used for compensating the arc bottom wall of the container liner 3, thereby forming a flat connecting plane, being convenient for the connection of the first connecting groove 502, and when the container liner 3 is positioned in the container liner 2, the spring 504 has a certain vertical upward acting force on the flat side wall, so that the container liner 3 is clamped between the container closure cap 4 and the fixing component 5, therefore, when the container closure cap 4 keeps the container liner 3 in a closed state, the container liner 3 is stably replaced in the container liner 2, and the container liner 3 is stably replaced in the container liner 2.
Referring to fig. 2, specifically, the lower end of the container closure 4 is fixedly connected with an annular clamping groove 9 for fixing the container liner 3, and when the container closure 4 is in a closed state, the upper ends of the container housing 2 and the container liner 3 are both located in the annular clamping groove 9, so that the annular clamping groove 9 has a fixing effect on the upper end of the container liner 3.
Referring to fig. 2, specifically, an annular compensating strip 10 equal to the height difference between the container liner 3 and the container shell 2 is disposed inside the annular clamping groove 9. The height of the container liner 3 is smaller than that of the container shell 2, and the annular compensation strip 10 is used for compensating the height difference between the container liner 3 and the container shell, so that the upper end of the container liner 3 is further fixed in an omnibearing manner.
Referring to fig. 2, specifically, a latch assembly 11 for fixing the container closure cap 4 is disposed on a side wall of the annular slot 9, and the latch assembly 11 is disposed such that the container closure cap 4 is locked at an opening at an upper end of the reaction container 1, so as to perform a sealing function on the reaction container 1.
Referring to fig. 2, specifically, the latch assembly 11 includes a symmetrically disposed connection block 111, a lock plate 112 is rotatably connected to the connection block 111, lock holes are formed in the lock plate 112 and on a side wall of the reaction vessel 1, a latch 113 is penetrated through the lock plate 112, the lock plate 112 can rotate under the action of an external force, and the latch 113 is fixed to the lock plate 112 and a lock hole formed in the side wall of the reaction vessel 1, so as to fix the lock plate 112, so that the vessel closing cover 4 is locked at an opening at an upper end of the reaction vessel 1, and performs a closing function on the reaction vessel 1.
Referring to fig. 2, specifically, the inside of the container closure 4 is of a cavity structure, the inside of the container closure 4 is provided with a reinforcing rib 12, the inside of the container closure 4 is of a cavity structure, so that the weight of the container closure 4 is reduced to a certain extent, the replacement of the container liner 3 inside is further facilitated, and the reinforcing rib 12 is used for reinforcing the strength of the container closure 4.
Referring to fig. 1, in particular, a material conveying pipe and a gas discharging pipe are provided on the container closure 4.
Referring to fig. 1 and 4, specifically, the main body of the evaporator 8 is a square tank, the inside of the evaporator 8 is uniformly provided with a spoiler set, the spoiler set is composed of two inclined panels 13 disposed in a vertical direction, the inclined panels 13 are square panels, one end of each inclined panel 13 is fixedly connected with the inner side wall of the evaporator 8, the free end of each inclined panel 13 is located at the upper side of the fixed end, the liquid phase part uniformly is provided with a spoiler set along the inside of the evaporator 8 from top to bottom, the liquid phase part flows along the inclined panels 13 layer by layer, and each liquid phase part needs to flow from bottom to top under the accumulation action of the rear freewheel due to the fact that the free end of each inclined panel 13 is located at the upper side of the fixed end, so that the circulation time of the liquid phase part in the evaporator 8 is effectively increased, the water and the polyaldehyde part in the liquid phase part are ensured to be evaporated completely, and the purity of acetic acid is improved.
Referring to fig. 1, a reaction process for preparing acetic acid by carbonylation of methanol comprises the following steps:
step 1: the catalyst solution is conveyed into the reaction vessel 1 through a material conveying pipe arranged on the vessel sealing cover 4, then gaseous carbon monoxide and gaseous methanol are conveyed into the reaction vessel 1 through a material conveying pipe arranged on the vessel sealing cover 4, the carbon monoxide and the gaseous methanol undergo methanol carbonylation reaction under the action of the catalyst to synthesize acetic acid and polyaldehyde, and the vessel liner 3 in the reaction vessel 1 is replaced periodically;
step 2: the liquid product in the reaction vessel 1 enters the flash tank 6 under the action of pump force, the gas in the reaction vessel 1 is discharged into the cooler 7 along the top, after the liquid product in the flash tank 6 is flashed, a gas phase part comprising a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde is discharged into the cooler 7 from the top of the flash tank, a liquid phase part enters the evaporator 8 for acetic acid purification treatment, after the gas in the cooler 7 is cooled, condensable liquid flows into the evaporator 8, non-condensable gas is discharged to an external absorption process, and the flash tank 6 and the cooler 7 finish primary separation of the product;
step 3: the liquid phase part from the flash tank 6 and the cooler 7 enters from the upper part of the evaporator 8, a flow blocking plate group uniformly flows from top to bottom along the inside of the evaporator 8, the temperature control inside the evaporator 8 is controlled at 100-105 ℃, water and multi-aldehyde part in the liquid phase part are gradually evaporated to be gas phase and discharged into an external collecting tank along the top of the evaporator 8, and the rest liquid phase part is acetic acid and discharged along the bottom of the evaporator 8.
In order that the objects and advantages of the invention will become more apparent, the invention will be further described with reference to the following examples; it should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
Acetic acid production was performed using the above system and process, wherein:
the inlet temperature of methanol and carbon monoxide is 160 ℃, the inlet pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of methanol to carbon monoxide is 1:1.
The temperature in the evaporator was 102 ℃.
After detection, the purity of the prepared acetic acid is 94% by using the system and the process.
Example 2
Acetic acid production was performed using the above system and process, wherein:
the inlet temperature of methanol and carbon monoxide is 160 ℃, the inlet pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of methanol to carbon monoxide is 1:1.
The temperature in the evaporator was 104 ℃.
After detection, the purity of the prepared acetic acid is 94% by using the system and the process.
Example 3
Acetic acid production was performed using the above system and process, wherein:
the inlet temperature of methanol and carbon monoxide is 160 ℃, the inlet pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of methanol to carbon monoxide is 1:1.
The temperature in the evaporator was 100 ℃.
After detection, the purity of the prepared acetic acid is 93% by using the system and the process.
Example 4
Acetic acid production was performed using the above system and process, wherein:
the inlet temperature of methanol and carbon monoxide is 160 ℃, the inlet pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of methanol to carbon monoxide is 1:1.
The temperature in the evaporator was 101 ℃.
After detection, the purity of the prepared acetic acid is 93% by using the system and the process.
Example 5
Acetic acid production was performed using the above system and process, wherein:
the inlet temperature of methanol and carbon monoxide is 160 ℃, the inlet pressure is 3.5Mpa, the temperature in the reactor is 170 ℃, the pressure is 3.8Mpa, and the ratio of the inlet air quantity of methanol to carbon monoxide is 1:1.
The temperature in the evaporator was 105 ℃.
After detection, the purity of the prepared acetic acid is 95% by using the system and the process.
Comparative example
The prior art process for the carbonylation of methanol to acetic acid was carried out using the same process parameters as in the examples above (excluding the evaporator section).
The purity of the finally prepared acetic acid was 83% by detection.
Thus far, the technical solution of the present invention has been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of protection of the present invention is not limited to these specific embodiments. Equivalent modifications and substitutions for related technical features may be made by those skilled in the art without departing from the principles of the present invention, and such modifications and substitutions will be within the scope of the present invention.
The foregoing description is only of the preferred embodiments of the invention and is not intended to limit the invention; various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A reaction system for preparing acetic acid by carbonylation of methanol, comprising:
the reaction vessel (1) is used for providing a reaction place for the carbonylation reaction of methanol, the reaction vessel (1) comprises a vessel shell (2), a vessel liner (3) and a vessel closing cover (4), the vessel liner (3) is positioned in the vessel shell (2), the inner wall of the vessel liner (3) replaces the vessel shell (2) to be contacted with reactants, and the vessel closing cover (4) is used for closing the open end of the reaction vessel (1);
the bottom wall of the container liner (3) is in a convex shape along the vertical upward direction, a reserved cavity (14) is formed between the bottom wall of the container liner (3) and the bottom wall of the container shell (2), and a fixing component (5) for fixing the container liner (3) is arranged in the reserved cavity (14);
a flash tank (6) which is in communication with the reaction vessel (1) and which performs flash separation of a product in the reaction vessel (1);
a cooler (7) which is communicated with the reaction vessel (1) and the flash tank (6) and is used for condensing the gas discharged from the top of the reaction vessel (1) and the gas discharged from the flash tank (6);
an evaporator (8) which is in communication with the flash tank (6) and the cooler (7) and which purifies the liquid product discharged from the flash tank (6) and the liquid product discharged from the cooler (7);
the fixing assembly (5) comprises a compensation plate (501), two symmetrical side walls on the compensation plate (501) are respectively an arc-surface side wall and a plane side wall, the arc-surface side wall of the compensation plate (501) is fixedly connected with the bottom wall of the container liner (3), a first connecting groove (502) and a second connecting groove (503) which are matched with each other are fixedly connected on the plane side wall of the compensation plate (501) and the inner bottom wall of the container shell (2), one end of a spring (504) is fixedly connected in the second connecting groove (503), and the other end of the spring (504) is connected with the first connecting groove (502) in a clamping mode.
2. The reaction system for preparing acetic acid by methanol carbonylation according to claim 1, wherein the lower end of the container closing cover (4) is fixedly connected with an annular clamping groove (9) for fixing the container liner (3).
3. Reaction system for the production of acetic acid by carbonylation of methanol according to claim 2, characterized in that the inside of the annular clamping groove (9) is provided with an annular compensating bar (10) equal to the difference in height between the container liner (3) and the container shell (2).
4. A reaction system for the carbonylation of methanol to acetic acid according to claim 3, wherein the side wall of the annular clamping groove (9) is provided with a locking assembly (11) for fixing the container closure cap (4).
5. The reaction system for preparing acetic acid by carbonylation of methanol according to claim 4, wherein the latch assembly (11) comprises symmetrically arranged connecting blocks (111), lock plates (112) are rotatably connected to the connecting blocks (111), lock holes are formed in the lock plates (112) and on the side walls of the reaction vessel (1), and lock bolts (113) penetrate through the lock plates (112).
6. The reaction system for preparing acetic acid by carbonylation of methanol according to any one of claims 1 to 5, wherein the inside of the container closure (4) is of a hollow structure, and the inside of the container closure (4) is provided with reinforcing ribs (12).
7. A reaction system for producing acetic acid by carbonylation of methanol according to claim 6, wherein a material feed pipe and a gas discharge pipe are both provided on the vessel closing cap (4).
8. The reaction system for preparing acetic acid by methanol carbonylation according to claim 1, wherein the main body of the evaporator (8) is a square tank, a spoiler group is uniformly arranged inside the evaporator (8), the spoiler group is composed of two inclined panels (13) arranged in the vertical direction, the inclined panels (13) are square panels, one end of each inclined panel (13) is fixedly connected with the inner side wall of the evaporator (8), and the free end of each inclined panel (13) is positioned on the upper side of the fixed end.
9. The reaction system for preparing acetic acid by carbonylation of methanol according to claim 1, wherein the preparation process comprises the steps of:
step 1: the catalyst solution is conveyed into the reaction vessel (1) through a material conveying pipe arranged on the vessel sealing cover (4), gaseous carbon monoxide and gaseous methanol are conveyed into the reaction vessel (1) through a material conveying pipe arranged on the vessel sealing cover (4), and the carbon monoxide and the gaseous methanol undergo methanol carbonylation reaction under the action of the catalyst to synthesize acetic acid and polyaldehyde, and the vessel liner (3) in the reaction vessel (1) is replaced periodically;
step 2: the liquid product in the reaction vessel (1) enters the flash tank (6) under the action of pump force, the gas in the reaction vessel (1) is discharged into the cooler (7) along the top, after the liquid product in the flash tank (6) is flashed, a gas phase part comprising a small amount of acetic acid, water, a small amount of catalyst components and multi-aldehyde is discharged into the cooler (7) from the top of the flash tank, a liquid phase part enters the evaporator (8) for acetic acid purification treatment, after the gas in the cooler (7) is cooled, the condensable liquid flows into the evaporator (8), the non-condensable gas is discharged to an external absorption process, and the flash tank (6) and the cooler (7) finish primary separation of the product;
step 3: the liquid phase part from the flash tank (6) and the cooler (7) enters from the upper part of the evaporator (8), a flow blocking plate group uniformly arranged in the liquid phase part along the interior of the evaporator (8) flows from top to bottom, the temperature control in the interior of the evaporator (8) is controlled at 100-105 ℃, water and multi-aldehyde part in the liquid phase part are gradually evaporated to form a gas phase and are discharged into an external collecting tank along the top of the evaporator (8), and the rest liquid phase part is acetic acid and is discharged along the bottom of the evaporator (8).
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