CN109627158B - Acetic anhydride joint production and separation method - Google Patents
Acetic anhydride joint production and separation method Download PDFInfo
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- CN109627158B CN109627158B CN201811509405.2A CN201811509405A CN109627158B CN 109627158 B CN109627158 B CN 109627158B CN 201811509405 A CN201811509405 A CN 201811509405A CN 109627158 B CN109627158 B CN 109627158B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/54—Preparation of carboxylic acid anhydrides
- C07C51/56—Preparation of carboxylic acid anhydrides from organic acids, their salts, their esters or their halides, e.g. by carboxylation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
Abstract
The invention discloses a combined production and separation method of acetic anhydride, which comprises the following steps: s1, synthesizing methyl acetate from methanol and acetic acid under normal pressure under the action of a sulfuric acid catalyst, wherein the reaction temperature is 65-85 ℃; s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 2.5-3Mpa and reaction temperature of 130-140 ℃ to generate acetic anhydride and CO-produce acetic acid. The invention has the advantages of prolonging the service life of the catalyst, reducing the reaction energy consumption and improving the reaction efficiency, and can be widely applied to the technical field of acetic anhydride combined production.
Description
Technical Field
The invention relates to the technical field of acetic anhydride joint production. More specifically, the invention relates to a combined production and separation method of acetic anhydride.
Background
In the prior art, when the CO-production of acetic acid and acetic anhydride is carried out by using a CO oxo synthesis method of methanol and acetic acid, the catalyst used in the second step is a rhodium catalyst, and the reaction temperature is between 140 and 160 ℃. The rhodium catalyst is expensive, and researches show that the service life of the catalyst is shortened at a higher reaction temperature. How to ensure the reaction efficiency of co-production when the reaction temperature is lower is an urgent problem to be solved.
Disclosure of Invention
The invention aims to provide a combined production and separation method of acetic anhydride, which can prolong the service life of a catalyst, reduce the reaction energy consumption and improve the reaction efficiency.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for co-producing and separating acetic anhydride, comprising:
s1, synthesizing methyl acetate from methanol and acetic acid under normal pressure under the action of a sulfuric acid catalyst, wherein the reaction temperature is 65-85 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 2.5-3Mpa and reaction temperature of 130-140 ℃ to generate acetic anhydride, CO-producing acetic acid, and separating to obtain acetic anhydride and acetic acid.
Preferably, the reaction kettle comprises:
a support platform horizontally arranged on the ground;
the two ends of the door-shaped bracket are fixed on the supporting platform;
the kettle body is arranged below the door-shaped bracket and comprises an upper kettle body and a lower kettle body; the lower kettle body is in a cylindrical shell shape without a top plate, an inner cavity of the lower kettle body is used for containing reaction liquid, the side wall of the lower kettle body is provided with a circular first inner hollow structure which is used for containing circulating water, the side wall of the lower kettle body is divided into an inner side wall and an outer side wall from inside to outside by the first inner hollow structure, and a water outlet and a water inlet which are communicated with the first inner hollow structure are arranged on the outer side wall of the lower kettle body; the upper kettle body is in a cylindrical shell shape without a bottom plate and matched with the inner cavity of the lower kettle body, and the lower part of the upper kettle body is seamlessly sleeved in the inner cavity of the upper part of the lower kettle body;
the non-telescopic ends of the pair of first electric telescopic rods are fixed at the transverse part of the door-shaped bracket, and the lower ends of the first electric telescopic rods are vertically downward and fixedly connected with a top plate of the upper kettle body;
the annular plate is sleeved and fixed at the top end of the outer wall of the upper kettle body;
the scraping cylinder is cylindrical and is sleeved and fixed outside the annular plate; the lower end of the scraping cylinder is flush with the lower end of the lower kettle body and extends into the first inner hollow structure of the lower accessory body, and the side wall of the scraping cylinder extending into the lower part of the first inner hollow structure is attached to the inner side wall and the outer side wall of the lower kettle body;
agitating unit, it includes second electric telescopic handle, and its non-flexible lower extreme is vertical to be fixed the center of the bottom plate upper surface of the cauldron body down, second electric telescopic handle's non-flexible lower extreme is fixed with a pair of relative and the level first stirring rake that sets up, second electric telescopic handle's flexible terminal surface relatively fixed has a pair of horizontally second stirring rake.
Preferably, the reaction kettle further comprises a gas rotary spraying device, which comprises:
the non-telescopic upper end of the third electric telescopic rod is fixed at the center of the top plate of the upper kettle body, the end surface of the telescopic end of the third electric telescopic rod is vertically downward and coaxially connected with the upper end of a vertical rod, at least one bearing is sleeved outside the vertical rod, the inner ring of the bearing is fixed with the vertical rod, a cylindrical sleeve rod is sleeved and fixed outside the bearing, and the outer part of the bearing is in a spiral stirring rod shape;
the interference stirring part is sleeved outside the lower end of the sleeve rod and is fixed on the inner wall of the lower part of the upper kettle body through a cross rod;
a disc-shaped air chamber is coaxially fixed on the end face of the lower end of the loop bar and is in a shape of a closed shell with a cylindrical inner cavity, and a bottom plate of the air chamber is sunken to form a plurality of air holes communicated with the inner cavity of the air chamber;
one end of the soft air pipe extends into the inner cavity of the kettle body and is communicated with the inner cavity of the air chamber;
when the third electric telescopic rod stretches, the vertical rod can be driven to move downwards or upwards, and the sleeve rod can rotate forwards or backwards in a circumferential direction under the interference of the interference stirring part.
Preferably, the bearings are a pair, and the pair of bearings is sleeved on the upper end and the lower end of the vertical rod respectively.
Preferably, the plurality of air holes are uniformly distributed on the bottom plate of the air chamber.
The invention at least comprises the following beneficial effects:
the acetic anhydride joint production and separation method provided by the invention has the advantages that the reaction temperature in the step S2 is controlled at 130-140 ℃, the energy consumption is saved, the service life of the rhodium catalyst is prolonged, the reaction liquid is fully contacted with CO, the reaction is thorough, the conversion rate of the reaction is improved, and the used reaction kettle is convenient to clean after the reaction is finished, so that the acetic anhydride joint production and separation method has the advantages of prolonging the service life of the catalyst, reducing the reaction energy consumption and having high reaction efficiency.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic structural view of a reaction kettle according to the present invention;
FIG. 2 is a schematic view of the connection relationship of the upper kettle body, the annular plate and the scraping cylinder;
FIG. 3 is a schematic view of the structure of the gas cell according to the present invention;
FIG. 4 is a schematic structural view of the lower kettle of the present invention.
Description of reference numerals: 1. a supporting table, 2, door type support, 3, go up the cauldron body, 4, the cauldron body down, 5, first electric telescopic handle, 6, the crown plate, 7, scrape a section of thick bamboo, 8, second electric telescopic handle, 9, first stirring rake, 10, second stirring rake, 11, third electric telescopic handle, 12, the montant, 13, the loop bar, 14, interfere stirring portion, 15, the horizontal pole, 16, the air chamber, 17, the gas pocket, 18, soft trachea, 19, the inner chamber of air chamber, 20, first interior hollow structure, 21, the inside wall of the cauldron body down, 22, the lateral wall of the cauldron body down.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials, if not otherwise specified, are commercially available; in the description of the present invention, the terms "lateral", "longitudinal", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
As shown in FIGS. 1-4, the present invention provides a combined production and separation method of acetic anhydride, comprising:
s1, synthesizing methyl acetate from methanol and acetic acid under normal pressure under the action of a sulfuric acid catalyst, wherein the reaction temperature is 65-85 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 2.5-3Mpa and reaction temperature of 130-140 ℃ to generate acetic anhydride, CO-producing acetic acid, and separating to obtain acetic anhydride and acetic acid.
In the technical scheme, the service life of the rhodium catalyst is prolonged by reducing the reaction temperature in the step S2, and meanwhile, the reaction liquid can be fully contacted with CO by using the modified reaction kettle at the temperature of 130-140 ℃, so that the reaction can be rapidly and completely carried out at a lower temperature.
In another aspect, the reaction vessel comprises:
a support table 1 horizontally arranged on the ground;
the two ends of the door-shaped bracket 2 are fixed on the supporting platform 1;
the kettle body is arranged below the door-shaped bracket 2 and comprises an upper kettle body 3 and a lower kettle body 4; the lower kettle body 4 is in a cylindrical shell shape without a top plate, an inner cavity of the lower kettle body 4 is used for containing reaction liquid, the side wall of the lower kettle body 4 is provided with a first annular inner hollow structure which is used for containing circulating water, the side wall of the lower kettle body 4 is divided into an inner side wall 21 and an outer side wall 22 from inside to outside by the first inner hollow structure, and a water outlet and a water inlet which are communicated with the first inner hollow structure are formed in the outer side wall 22 of the lower kettle body 4; the upper kettle body 3 is in a cylindrical shell shape without a bottom plate and matched with the inner cavity of the lower kettle body 4, and the lower part of the upper kettle body 3 is seamlessly sleeved in the inner cavity of the upper part of the lower kettle body 4;
a pair of first electric telescopic rods 5, the non-telescopic ends of which are fixed at the transverse part of the door-shaped bracket 2, and the lower ends of the first electric telescopic rods 5 are vertically downward and fixedly connected with a top plate of the upper kettle body 3;
the annular plate 6 is sleeved and fixed at the top end of the outer wall of the upper kettle body 3;
the scraping cylinder 7 is cylindrical and is sleeved and fixed outside the annular plate 6; the lower end of the scraping cylinder 7 is flush with the lower end of the lower kettle body 4 and extends into the first inner hollow structure of the lower accessory body, and the side wall of the lower part of the scraping cylinder 7 extending into the first inner hollow structure is attached to the inner side wall and the outer side wall of the lower kettle body 4;
agitating unit, it includes second electric telescopic handle 8, and its non-flexible lower extreme is vertical to be fixed the center of the bottom plate upper surface of cauldron body 4 down, the non-flexible lower extreme of second electric telescopic handle 8 is fixed with a pair of relative and the level first stirring rake 9 that sets up, the flexible terminal surface relatively fixed of second electric telescopic handle 8 has a pair of horizontally second stirring rake 10.
In this kind of technical scheme, first interior hollow structure is used for holding water with temperature in the first interior hollow structure 20 to come to carry out heat transfer to the reaction liquid in the cauldron body 4 downwards, thereby guarantee reaction temperature.
Through setting up a pair of first stirring rake 9 and a pair of second stirring rake 10 for hold the reaction liquid of the inner chamber of cauldron body 4 under by intensive mixing, and can adjust the height of second stirring rake 10 through second electric telescopic handle 8 according to the liquid level height of reaction liquid, prevent that second stirring rake 10 from idle running. Moreover, the upper kettle body 3 of the reaction kettle is sleeved in the lower kettle body 4, and after the reaction is finished, the outer wall of the upper kettle body 3 can continuously scrape solid matters attached to the inner side of the inner side wall of the lower kettle body 4 through the extension and retraction of the pair of first electric telescopic rods 5, so that the lower kettle body 4 can be conveniently cleaned; it drives rather than the scraping section of thick bamboo 7 up-and-down motion of fixed connection when last cauldron body 3 moves from top to bottom to the inboard of the lateral wall of cauldron body 4 will be down and the outside of inside wall is constantly scraped, prevents that the incrustation scale from condensing, influences heat transfer effect.
The lower kettle body 4 is also provided with a reaction liquid inlet and a reaction liquid outlet. The reaction liquid inlet and the reaction liquid outlet can be opened and closed, so that the sealing property of the kettle body is ensured. The outer wall of the upper kettle body and the inner wall of the lower kettle body are well sealed, so that the sealing performance of the kettle body is guaranteed, and sealing rubber can be arranged between the outer wall of the upper kettle body and the inner wall of the lower kettle body, so that the sealing performance is improved. The water outlet and the water inlet of the circulating water on the lower kettle body can be opened and closed.
In another technical scheme, the reaction kettle further comprises a gas rotary spraying device, which comprises:
the non-telescopic upper end of the third electric telescopic rod 11 is fixed at the center of the top plate of the upper kettle body 3, the end face of the telescopic end of the third electric telescopic rod 11 is vertically downward and coaxially connected with the upper end of a vertical rod 12, at least one bearing is sleeved outside the vertical rod 12, the inner ring of the bearing is fixed with the vertical rod 12, a cylindrical sleeve rod 13 is sleeved and fixed outside the bearing, and the outer part of the bearing is in a spiral stirring rod shape;
the interference stirring part 14 is sleeved outside the lower end of the loop bar 13, and the interference stirring part 14 is fixed on the inner wall of the lower part of the upper kettle body 3 through a cross bar 15;
a disc-shaped air chamber 16 is coaxially fixed on the lower end face of the loop bar 13, and is in a closed shell shape with a cylindrical inner cavity 19, and a bottom plate of the air chamber 16 is sunken to form a plurality of air holes 17 communicated with the inner cavity 19;
one end of the soft air pipe 18 extends into the inner cavity of the kettle body and is communicated with the inner cavity of the air chamber 16;
when the third electric telescopic rod 11 is extended, the vertical rod 12 can be driven to move downwards or upwards, and the loop bar 13 can rotate in a circumferential forward or reverse direction under the interference of the interference stirring part 14.
In this kind of technical scheme, third electric telescopic handle 11 stretches out the back, can make the air chamber 16 get into below the liquid level of reaction liquid from the liquid level top of reaction liquid to at the decline in-process, thereby air chamber 16 can be round its axle to move round and form and make CO spout the inside effect of each height of reaction liquid soon, make CO and reaction liquid contact more abundant, thereby guarantee more thoroughly of reaction, guarantee the conversion rate of reaction. The other end of the soft air pipe 18, which is far away from the air chamber 16, is positioned outside the reaction kettle and is communicated with an air storage tank for storing CO. The length of the soft air pipe 18 in the reaction kettle does not limit the extension of the third telescopic rod. The interference stirring portion 14 may be a square cylinder structure, when the third electric telescopic rod 11 extends, the vertical rod 12 is driven to move downward or upward, so as to drive the loop bar 13 to move downward or upward, and the spiral structure outside the loop bar 13 can rotate in a forward or reverse direction while descending or ascending under the interference of the interference stirring portion 14.
In another technical scheme, the pair of bearings is sleeved on the upper end and the lower end of the vertical rod 12 respectively.
In this kind of technical scheme, it is more stable to use a pair of bearing.
In another technical solution, a plurality of air holes 17 are uniformly distributed on the bottom plate of the air chamber 16.
The uniform distribution of the air holes 17 ensures that the air distribution of the CO in the reaction liquid is more uniform by the air chamber 16.
Example one
S1, synthesizing methyl acetate from methanol and acetic acid under the action of a sulfuric acid catalyst at normal pressure, wherein the reaction temperature is 65 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 2.5Mpa and reaction temperature of 130 ℃ to generate acetic anhydride and CO-produce acetic acid, and separating to obtain acetic anhydride and acetic acid.
Example two
S1, synthesizing methyl acetate from methanol and acetic acid under the action of a sulfuric acid catalyst at normal pressure, wherein the reaction temperature is 75 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 2.75Mpa and reaction temperature of 135 ℃ to generate acetic anhydride and CO-produce acetic acid, and separating to obtain acetic anhydride and acetic acid.
EXAMPLE III
S1, synthesizing methyl acetate from methanol and acetic acid under the action of a sulfuric acid catalyst at normal pressure, wherein the reaction temperature is 85 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 3Mpa and reaction temperature of 140 ℃ to generate acetic anhydride, CO-producing acetic acid, and separating to obtain acetic anhydride and acetic acid.
Examples one to three reaction vessels used all included:
a support platform horizontally arranged on the ground;
the two ends of the door-shaped bracket are fixed on the supporting platform;
the kettle body is arranged below the door-shaped bracket and comprises an upper kettle body and a lower kettle body; the lower kettle body is in a cylindrical shell shape without a top plate, an inner cavity of the lower kettle body is used for containing reaction liquid, the side wall of the lower kettle body is provided with a circular first inner hollow structure which is used for containing circulating water, the side wall of the lower kettle body is divided into an inner side wall and an outer side wall from inside to outside by the first inner hollow structure, and a water outlet and a water inlet which are communicated with the first inner hollow structure are arranged on the outer side wall of the lower kettle body; the upper kettle body is in a cylindrical shell shape without a bottom plate and matched with the inner cavity of the lower kettle body, and the lower part of the upper kettle body is seamlessly sleeved in the inner cavity of the upper part of the lower kettle body;
the non-telescopic ends of the pair of first electric telescopic rods are fixed at the transverse part of the door-shaped bracket, and the lower ends of the first electric telescopic rods are vertically downward and fixedly connected with a top plate of the upper kettle body;
the annular plate is sleeved and fixed at the top end of the outer wall of the upper kettle body;
the scraping cylinder is cylindrical and is sleeved and fixed outside the annular plate; the lower end of the scraping cylinder is flush with the lower end of the lower kettle body and extends into the first inner hollow structure of the lower accessory body, and the side wall of the scraping cylinder extending into the lower part of the first inner hollow structure is attached to the inner side wall and the outer side wall of the lower kettle body;
agitating unit, it includes second electric telescopic handle, and its non-flexible lower extreme is vertical to be fixed the center of the bottom plate upper surface of the cauldron body down, second electric telescopic handle's non-flexible lower extreme is fixed with a pair of relative and the level first stirring rake that sets up, second electric telescopic handle's flexible terminal surface relatively fixed has a pair of horizontally second stirring rake.
The reation kettle still includes gaseous rotary spraying device, and it includes:
the non-telescopic upper end of the third electric telescopic rod is fixed at the center of the top plate of the upper kettle body, the end surface of the telescopic end of the third electric telescopic rod is vertically downward and coaxially connected with the upper end of a vertical rod, at least one bearing is sleeved outside the vertical rod, the inner ring of the bearing is fixed with the vertical rod, a cylindrical sleeve rod is sleeved and fixed outside the bearing, and the outer part of the bearing is in a spiral stirring rod shape;
the interference stirring part is sleeved outside the lower end of the sleeve rod and is fixed on the inner wall of the lower part of the upper kettle body through a cross rod;
a disc-shaped air chamber is coaxially fixed on the end face of the lower end of the loop bar and is in a shape of a closed shell with a cylindrical inner cavity, and a bottom plate of the air chamber is sunken to form a plurality of air holes communicated with the inner cavity of the air chamber;
one end of the soft air pipe extends into the inner cavity of the kettle body and is communicated with the inner cavity of the air chamber;
when the third electric telescopic rod stretches, the vertical rod can be driven to move downwards or upwards, and the sleeve rod can rotate forwards or backwards in a circumferential direction under the interference of the interference stirring part.
The bearing is a pair, and a pair of bearings is respectively sleeved at the upper end and the lower end of the vertical rod.
The air holes are uniformly distributed on the bottom plate of the air chamber.
Comparative example:
s1, synthesizing methyl acetate from methanol and acetic acid under the action of a sulfuric acid catalyst at normal pressure, wherein the reaction temperature is 85 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 3Mpa and reaction temperature of 140 ℃ to generate acetic anhydride, CO-producing acetic acid, and separating to obtain acetic anhydride and acetic acid. Wherein the reaction kettle is a conventional reaction kettle.
The test results of examples one to three are compared with those of the comparative example as follows:
(01) the following are the mean values of the experimental data obtained in examples one to three:
the selectivity of the acid anhydride of the carbonylation product calculated according to CO is 96.1%, the conversion rate of CO is 98%, the yield of the acid anhydride of the carbonylation product is 93.4%, the selectivity of the acid anhydride calculated according to methanol is 93.8%, the conversion rate of the methanol is 97.5%, the yield of the acid anhydride of the carbonylation product is 92.3%, the selectivity of the acid anhydride calculated according to methyl acetate is 89.6%, the conversion rate of the methyl acetate is 65%, and the yield of the acid anhydride of the carbonylation product is 85%.
(02) The average of the experimental data of three consecutive replicates of the comparative example is as follows:
the selectivity of the acid anhydride of the carbonylation product calculated according to CO is 93.9%, the conversion rate of CO is 95.6%, the yield of the acid anhydride of the carbonylation product is 91.3%, the selectivity of the acid anhydride calculated according to methanol is 89.5%, the conversion rate of the methanol is 92.5%, the yield of the acid anhydride of the carbonylation product is 90.3%, the selectivity of the acid anhydride calculated according to methyl acetate is 87.6%, the conversion rate of the methyl acetate is 60.7%, and the yield of the acid anhydride of the carbonylation product is 83%.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (3)
1. The acetic anhydride joint production and separation method is characterized by comprising the following steps:
s1, synthesizing methyl acetate from methanol and acetic acid under normal pressure under the action of a sulfuric acid catalyst, wherein the reaction temperature is 65-85 ℃;
s2, adding methyl acetate and methanol into a reaction kettle, introducing CO, reacting under the action of potassium iodide and rhodium catalyst under the conditions of reaction pressure of 2.5-3Mpa and reaction temperature of 130-140 ℃ to generate acetic anhydride, CO-producing acetic acid, and separating to obtain acetic anhydride and acetic acid;
the reaction kettle comprises:
a support platform horizontally arranged on the ground;
the two ends of the door-shaped bracket are fixed on the supporting platform;
the kettle body is arranged below the door-shaped bracket and comprises an upper kettle body and a lower kettle body; the lower kettle body is in a cylindrical shell shape without a top plate, an inner cavity of the lower kettle body is used for containing reaction liquid, the side wall of the lower kettle body is provided with a circular first inner hollow structure which is used for containing circulating water, the side wall of the lower kettle body is divided into an inner side wall and an outer side wall from inside to outside by the first inner hollow structure, and a water outlet and a water inlet which are communicated with the first inner hollow structure are arranged on the outer side wall of the lower kettle body; the upper kettle body is in a cylindrical shell shape without a bottom plate and matched with the inner cavity of the lower kettle body, and the lower part of the upper kettle body is seamlessly sleeved in the inner cavity of the upper part of the lower kettle body;
the non-telescopic ends of the pair of first electric telescopic rods are fixed at the transverse part of the door-shaped bracket, and the lower ends of the first electric telescopic rods are vertically downward and fixedly connected with a top plate of the upper kettle body;
the annular plate is sleeved and fixed at the top end of the outer wall of the upper kettle body;
the scraping cylinder is cylindrical and is sleeved and fixed outside the annular plate; the lower end of the scraping cylinder is flush with the lower end of the lower kettle body and extends into the first inner hollow structure of the lower kettle body, and the side wall of the lower part of the scraping cylinder extending into the first inner hollow structure is attached to the inner side wall and the outer side wall of the lower kettle body;
the stirring device comprises a second electric telescopic rod, the non-telescopic lower end of the second electric telescopic rod is vertically fixed at the center of the upper surface of the bottom plate of the lower kettle body, a pair of first stirring paddles which are oppositely and horizontally arranged are fixed at the non-telescopic lower end of the second electric telescopic rod, and a pair of second horizontal stirring paddles are oppositely fixed at the telescopic end surface of the second electric telescopic rod;
the reation kettle still includes gaseous rotary spraying device, and it includes:
the non-telescopic upper end of the third electric telescopic rod is fixed at the center of the top plate of the upper kettle body, the end surface of the telescopic end of the third electric telescopic rod is vertically downward and coaxially connected with the upper end of a vertical rod, at least one bearing is sleeved outside the vertical rod, the inner ring of the bearing is fixed with the vertical rod, a cylindrical sleeve rod is sleeved and fixed outside the bearing, and the outer part of the bearing is in a spiral stirring rod shape;
the interference stirring part is sleeved outside the lower end of the sleeve rod and is fixed on the inner wall of the lower part of the upper kettle body through a cross rod;
a disc-shaped air chamber is coaxially fixed on the end face of the lower end of the loop bar and is in a shape of a closed shell with a cylindrical inner cavity, and a bottom plate of the air chamber is sunken to form a plurality of air holes communicated with the inner cavity of the air chamber;
one end of the soft air pipe extends into the inner cavity of the kettle body and is communicated with the inner cavity of the air chamber;
when the third electric telescopic rod stretches, the vertical rod can be driven to move downwards or upwards, and the sleeve rod can rotate forwards or backwards in a circumferential direction under the interference of the interference stirring part.
2. The joint production and separation method of acetic anhydride as claimed in claim 1, wherein the pair of bearings are provided, and the pair of bearings are respectively fitted over the upper and lower ends of the vertical rod.
3. The process for co-producing and separating acetic anhydride according to claim 1, wherein the plurality of pores are uniformly distributed on the bottom plate of the gas chamber.
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