CN109627158A - Acetic acid aceticanhydride Joint Production and separation method - Google Patents
Acetic acid aceticanhydride Joint Production and separation method Download PDFInfo
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- CN109627158A CN109627158A CN201811509405.2A CN201811509405A CN109627158A CN 109627158 A CN109627158 A CN 109627158A CN 201811509405 A CN201811509405 A CN 201811509405A CN 109627158 A CN109627158 A CN 109627158A
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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
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of acetic acid aceticanhydride Joint Production and separation methods, comprising: S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 65-85 DEG C；S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in reaction pressure 2.5-3Mpa, under conditions of reaction temperature is 130-140 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid.The present invention, which has, delays catalyst service life, reduces energy consumption of reaction, improves the high advantage of reaction efficiency, can be widely applied to acetic acid aceticanhydride Joint Production technical field.
Description
Technical field
The present invention relates to acetic acid aceticanhydride Joint Production technical fields.It is more particularly related to a kind of acetic acid aceticanhydride
Joint Production and separation method.
Background technique
In the prior art, when carrying out coproduction by acetic acid, aceticanhydride using the CO oxo synthesis of methanol, acetic acid, second step makes
Catalyst is rhodium series catalysts, and reaction temperature is between 140 DEG C -160 DEG C.Rhodium series catalysts price is somewhat expensive, studies table
It is bright its in high reaction temperatures, service life can shorten.How when reaction temperature is lower, the reaction effect of coproduction can guarantee
Rate is a urgent problem.
Summary of the invention
It can delay catalyst service life the object of the present invention is to provide a kind of, reduce energy consumption of reaction, improve reaction efficiency
High acetic acid aceticanhydride Joint Production and separation method.
In order to realize these purposes and other advantages according to the present invention, provide a kind of acetic acid aceticanhydride Joint Production and point
From method, comprising:
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 65-85 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in anti-
Answer pressure 2.5-3Mpa, under conditions of reaction temperature is 130-140 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid, by point
From obtaining aceticanhydride and acetic acid.
Preferably, the reaction kettle includes:
Supporting table is horizontally placed on ground；
Door shaped stent, both ends are fixed on the supporting table；
Autoclave body is arranged below door shaped stent, and the autoclave body includes upper kettle and lower kettle；The lower kettle is no top
The cylindrical housings shape of plate, the inner cavity of the lower kettle have circular for accommodating reaction solution, the side wall of the lower kettle
Hollow structure in first is used to accommodate recirculated water, in described first hollow structure by the side wall of the lower kettle be divided by
Interior to outer inner sidewall and lateral wall, be provided on the lateral wall of the lower kettle with described first in hollow structure perforation go out
The mouth of a river and water inlet；The upper kettle is cylindrical housings shape cooperate with the inner cavity of the lower kettle, without bottom plate, it is described on
The lower part of autoclave body is seamless to be sheathed on the inner cavity on the lower kettle top；
A pair of first electric telescopic rod, non-telescoping end are fixed on the lateral part of the door shaped stent, first electricity
The lower end of dynamic telescopic rod straight down and is fixedly connected with the top plate of the upper kettle；
Ring flat-plate is arranged and is fixed on the top of the outer wall of the upper kettle；
Cylinder is scraped, is tubular, and is arranged and is fixed on outside the ring flat-plate；Under the lower end for scraping cylinder and the lower kettle
Hold level with both hands it is neat, and stretch to it is described under attached body first in hollow structure, it is described to scrape the protruding into first under hollow structure of cylinder
The side wall in portion is bonded the inside and outside side wall of the lower kettle；
Agitating device comprising the second electric telescopic rod, non-telescoping lower end are fixed on the bottom plate of the lower kettle vertically
The center of upper surface, the non-telescoping lower end of the second electric telescopic rod are fixed with a pair of opposite and horizontally disposed first agitating paddle,
Relatively fixed the second agitating paddle for having a pair of of level in the flexible end face of second electric telescopic rod.
Preferably, the reaction kettle further includes gas whirl spraying device comprising:
Third electric telescopic rod, non-telescoping upper end are fixed on the center of the top plate of the upper kettle, and the third is electronic
The end face vertical of the telescopic end of telescopic rod is downward and the upper end of a coaxially connected vertical bar, the outer cover of the vertical bar are equipped at least one
Bearing, the inner ring of bearing are fixed with the vertical bar, and the outside of the bearing is arranged and is fixed with a cylindric loop bar, outside
It is rodlike for auger；
Interfere mixing part, is set in the outside of the lower end of the loop bar, the interference mixing part is fixed by a cross bar
On the inner wall of the lower part of the upper kettle；
The lower end surface of the loop bar is coaxially fixed with a disk-shaped gas chamber, is the closed housing with cylindrical lumens
Body shape, the bottom plate of the gas chamber invaginate to form multiple stomatas communicated with its inner cavity；
Soft tracheae, one end protrude into the inner cavity of the autoclave body, and are connected to the inner cavity of the gas chamber；
Wherein, when the third electric telescopic rod is flexible, the vertical bar can be driven to move downward or upward, the loop bar
It is described interference mixing part interference under can circumference forward or reverse.
Preferably, the bearing is a pair, and a pair of bearings is respectively sleeved at the upper and lower end of the vertical bar.
Preferably, multiple stomatas are evenly distributed on the bottom plate of the gas chamber.
The present invention is include at least the following beneficial effects:
Acetic acid aceticanhydride Joint Production provided by the invention and separation method are by existing the reaction temperature control of step S2
130-140 DEG C, not only save energy consumption, while having delayed the service life of rhodium series catalysts, at the same by make reaction solution with
CO comes into full contact with, and ensure that the thorough of reaction, and the reaction kettle for improving the conversion ratio of reaction, and using is convenient for after the reaction was completed
Cleaning, therefore the present invention be it is a kind of can delay catalyst service life, reduce energy consumption of reaction, the high acetic acid aceticanhydride connection of reaction efficiency
Symphysis production and separation method.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of reaction kettle of the present invention；
Fig. 2 is upper kettle of the present invention, ring flat-plate, the connection relationship diagram for scraping cylinder；
Fig. 3 is the structural schematic diagram of gas chamber of the present invention；
Fig. 4 is the structural schematic diagram of lower kettle of the present invention.
Description of symbols: 1, supporting table, 2, door shaped stent, 3, upper kettle, 4, lower kettle, the 5, first electric telescopic rod,
6, ring flat-plate, 7, scrape cylinder, the 8, second electric telescopic rod, the 9, first agitating paddle, the 10, second agitating paddle, 11, third electric telescopic rod,
12, vertical bar, 13, loop bar, 14, interference mixing part, 15, cross bar, 16, gas chamber, 17, stomata, 18, soft tracheae, 19, gas chamber it is interior
Chamber, hollow structure in 20, first, 21, the inner sidewall of lower kettle, 22, the lateral wall of lower kettle.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained；In the description of the present invention, term " transverse direction ", " vertical
To ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", the instructions such as "outside" side
Position or positional relationship are to be based on the orientation or positional relationship shown in the drawings, and are merely for convenience of description of the present invention and simplification of the description,
It is not that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, because
This is not considered as limiting the invention.
As shown in Figs 1-4, the present invention provides a kind of acetic acid aceticanhydride Joint Production and separation method, comprising:
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 65-85 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in anti-
Answer pressure 2.5-3Mpa, under conditions of reaction temperature is 130-140 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid, by point
From obtaining aceticanhydride and acetic acid.
In this kind of technical solution, the present invention extends making for rhodium series catalysts by the reaction temperature of reduction step S2
With the service life, while by using the reaction kettle by being transformed, under conditions of 130-140 DEG C, reaction solution can more sufficiently and CO
Contact guarantees under lower temperature that reaction also quickly, can be carried out thoroughly.
In another technical solution, the reaction kettle includes:
Supporting table 1, is horizontally placed on ground；
Door shaped stent 2, both ends are fixed in the supporting table 1；
Autoclave body is arranged below door shaped stent 2, and the autoclave body includes upper kettle 3 and lower kettle 4；The lower kettle 4 is
The cylindrical housings shape of no-top plate, the inner cavity of the lower kettle 4 have circle for accommodating reaction solution, the side wall of the lower kettle 4
Hollow structure in cricoid first is used to accommodate recirculated water, and hollow structure divides the side wall of the lower kettle 4 in described first
Be divided into inner sidewall 21 and lateral wall 22 from the inside to the outside, be provided on the lateral wall 22 of the lower kettle 4 with described first in
The water outlet and water inlet of hollow structure perforation；The upper kettle 3 is circle cooperate with the inner cavity of the lower kettle 4, without bottom plate
Cylindrical shell shape, the lower part of the upper kettle 3 is seamless to be sheathed on the inner cavity on 4 top of lower kettle；
A pair of first electric telescopic rod 5, non-telescoping end are fixed on the lateral part of the door shaped stent 2, and described first
The lower end of electric telescopic rod 5 straight down and is fixedly connected with the top plate of the upper kettle 3；
Ring flat-plate 6 is arranged and is fixed on the top of the outer wall of the upper kettle 3；
Cylinder 7 is scraped, is tubular, and is arranged and is fixed on outside the ring flat-plate 6；The lower end for scraping cylinder 7 and the lower kettle 4
Lower end it is concordant, and stretch to it is described under attached body first in hollow structure, it is described scrape cylinder 7 protrude into hollow structure in first
The side wall of lower part be bonded the inside and outside side wall of the lower kettle 4；
Agitating device comprising the second electric telescopic rod 8, non-telescoping lower end are fixed on the bottom of the lower kettle 4 vertically
The center of plate upper surface, the non-telescoping lower end of the second electric telescopic rod 8 are fixed with a pair of opposite and horizontally disposed first stirring
Paddle 9, relatively fixed the second agitating paddle 10 for having a pair of of level in the flexible end face of second electric telescopic rod 8.
In this kind of technical solution, temperature is had for accommodating in hollow structure 20 in hollow structure first in first
Water, to conduct heat come the reaction solution into lower kettle 4, to guarantee reaction temperature.
By the way that a pair of first agitating paddle 9 and a pair of second agitating paddle 10 is arranged, so that being contained in the anti-of the inner cavity of lower kettle 4
It answers liquid to be sufficiently agitated, and the second agitating paddle can be adjusted by the second electric telescopic rod 8 according to the liquid level of reaction solution
10 height prevents the second agitating paddle 10 from dallying.Also, the upper kettle 3 of the reaction kettle is set in lower kettle 4, when having reacted
Cheng Hou, can be by the flexible of a pair of first electric telescopic rod 5, so that the outer wall of upper kettle 3 constantly strikes off the inside of lower kettle 4
The solid content adhered on the inside of wall is convenient to clean lower kettle 4；It drives the company of being secured to while about 3 upper kettle is dynamic
What is connect scrapes the up and down motion of cylinder 7, so that the inside of the lateral wall of lower kettle 4 and the outside of inner sidewall constantly be scraped, prevents scale
Condensation, influences heat-transfer effect.
Lower kettle 4 is additionally provided with reaction solution import and reaction solution outlet.The reaction solution import, reaction solution outlet be can
Folding, to guarantee the leakproofness of autoclave body.The outer wall of upper kettle and the good seal between lower kettle inner wall, to guarantee autoclave body
Leakproofness, seal rubber can also be set in the outer wall of upper kettle and between lower kettle inner wall, to improve leakproofness.Lower kettle
The water outlet and water inlet of recirculated water on body are retractable.
In another technical solution, the reaction kettle further includes gas whirl spraying device comprising:
Third electric telescopic rod 11, non-telescoping upper end are fixed on the center of the top plate of the upper kettle 3, the third electricity
The end face vertical of the telescopic end of dynamic telescopic rod 11 is downward and the upper end of a coaxially connected vertical bar 12, and the outside of the vertical bar 12 is arranged
There is an at least bearing, the inner ring of bearing and the vertical bar 12 are fixed, and the outside of the bearing is arranged and is fixed with a cylindrical shape
Loop bar 13, external is that auger is rodlike；
Interfere mixing part 14, be set in the outside of the lower end of the loop bar 13, the interference mixing part 14 is horizontal by one
Bar 15 is fixed on the inner wall of the lower part of the upper kettle 3；
The lower end surface of the loop bar 13 is coaxially fixed with a disk-shaped gas chamber 16, for cylindrical lumens 19
Closed housing shape, the bottom plate of the gas chamber 16 invaginate to form multiple stomatas 17 communicated with its inner cavity 19；
Soft tracheae 18, one end protrude into the inner cavity of the autoclave body, and are connected to the inner cavity of the gas chamber 16；
Wherein, when the third electric telescopic rod 11 is stretched, the vertical bar 12 can be driven to move downward or upward, it is described
Loop bar 13 it is described interference mixing part 14 interference under can circumference forward or reverse.
In this kind of technical solution, after third electric telescopic rod 11 is stretched out, it may make gas chamber 16 from the liquid level of reaction solution
Side enter the liquid level of reaction solution hereinafter, and during decline, gas chamber 16 can be around its axis circular-rotation to being formed such that
CO whirl spraying enters the effect of each height inside reaction solution so that CO contact with reaction solution it is more abundant, to guarantee to react more
Thoroughly, guarantee the conversion ratio of reaction.The soft tracheae 18 is located on the outside of reaction kettle and connects far from the other end of the gas chamber 16
It is connected with the air accumulator for being stored with CO.Length of the soft tracheae 18 in reaction kettle, without limitation on the flexible of third telescopic rod.It is described
Interference mixing part 14 may be configured as square tube shape structure, when the third electric telescopic rod 11 is stretched, drive the vertical bar 12 to
Lower or upward, to drive the loop bar 13 downward or upward, the spiral helicine structure outside loop bar 13 is in interference mixing part 14
Interference under, while down or up can circumference forward or reverse.
In another technical solution, the bearing is a pair, and a pair of bearings is respectively sleeved at the upper and lower of the vertical bar 12
End.
It is more stable using a pair of bearings in this kind of technical solution.
In another technical solution, multiple stomatas 17 are evenly distributed on the bottom plate of the gas chamber 16.
Stomata 17 is uniformly distributed so that gas chamber 16 is more uniform to gas distribution of the CO in reaction solution.
Embodiment one
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 65 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in anti-
It answers pressure 2.5Mpa, under conditions of reaction temperature is 130 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid, by isolated
Aceticanhydride and acetic acid.
Embodiment two
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 75 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in anti-
It answers pressure 2.75Mpa, under conditions of reaction temperature is 135 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid, by separating
To aceticanhydride and acetic acid.
Embodiment three
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 85 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in anti-
It answers pressure 3Mpa, under conditions of reaction temperature is 140 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid passes through isolated vinegar
Acid anhydride and acetic acid.
The reaction kettle that embodiment one to three uses includes:
Supporting table is horizontally placed on ground；
Door shaped stent, both ends are fixed on the supporting table；
Autoclave body is arranged below door shaped stent, and the autoclave body includes upper kettle and lower kettle；The lower kettle is no top
The cylindrical housings shape of plate, the inner cavity of the lower kettle have circular for accommodating reaction solution, the side wall of the lower kettle
Hollow structure in first is used to accommodate recirculated water, in described first hollow structure by the side wall of the lower kettle be divided by
Interior to outer inner sidewall and lateral wall, be provided on the lateral wall of the lower kettle with described first in hollow structure perforation go out
The mouth of a river and water inlet；The upper kettle is cylindrical housings shape cooperate with the inner cavity of the lower kettle, without bottom plate, it is described on
The lower part of autoclave body is seamless to be sheathed on the inner cavity on the lower kettle top；
A pair of first electric telescopic rod, non-telescoping end are fixed on the lateral part of the door shaped stent, first electricity
The lower end of dynamic telescopic rod straight down and is fixedly connected with the top plate of the upper kettle；
Ring flat-plate is arranged and is fixed on the top of the outer wall of the upper kettle；
Cylinder is scraped, is tubular, and is arranged and is fixed on outside the ring flat-plate；Under the lower end for scraping cylinder and the lower kettle
Hold level with both hands it is neat, and stretch to it is described under attached body first in hollow structure, it is described to scrape the protruding into first under hollow structure of cylinder
The side wall in portion is bonded the inside and outside side wall of the lower kettle；
Agitating device comprising the second electric telescopic rod, non-telescoping lower end are fixed on the bottom plate of the lower kettle vertically
The center of upper surface, the non-telescoping lower end of the second electric telescopic rod are fixed with a pair of opposite and horizontally disposed first agitating paddle,
Relatively fixed the second agitating paddle for having a pair of of level in the flexible end face of second electric telescopic rod.
The reaction kettle further includes gas whirl spraying device comprising:
Third electric telescopic rod, non-telescoping upper end are fixed on the center of the top plate of the upper kettle, and the third is electronic
The end face vertical of the telescopic end of telescopic rod is downward and the upper end of a coaxially connected vertical bar, the outer cover of the vertical bar are equipped at least one
Bearing, the inner ring of bearing are fixed with the vertical bar, and the outside of the bearing is arranged and is fixed with a cylindric loop bar, outside
It is rodlike for auger；
Interfere mixing part, is set in the outside of the lower end of the loop bar, the interference mixing part is fixed by a cross bar
On the inner wall of the lower part of the upper kettle；
The lower end surface of the loop bar is coaxially fixed with a disk-shaped gas chamber, is the closed housing with cylindrical lumens
Body shape, the bottom plate of the gas chamber invaginate to form multiple stomatas communicated with its inner cavity；
Soft tracheae, one end protrude into the inner cavity of the autoclave body, and are connected to the inner cavity of the gas chamber；
Wherein, when the third electric telescopic rod is flexible, the vertical bar can be driven to move downward or upward, the loop bar
It is described interference mixing part interference under can circumference forward or reverse.
The bearing is a pair, and a pair of bearings is respectively sleeved at the upper and lower end of the vertical bar.
Multiple stomatas are evenly distributed on the bottom plate of the gas chamber.
Comparative example:
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 85 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in anti-
It answers pressure 3Mpa, under conditions of reaction temperature is 140 DEG C, carries out reaction and generate aceticanhydride, co-production acetic acid passes through isolated vinegar
Acid anhydride and acetic acid.Wherein, reaction kettle is conventional reactor.
Embodiment one to three and the comparison of test results of comparative example are as follows:
(01) mean value of the test data obtained the following are embodiment one to embodiment three:
Carbonylation product is calculated by CO, and acid anhydrides is selectively that 96.1%, CO conversion ratio is 98%, carbonyl products acid anhydrides yield
It is 93.4%, is calculated by methanol, acid anhydrides is selectively 93.8%, methanol conversion 97.5%, carbonylation product acid anhydrides yield
It is 92.3%, is calculated by methyl acetate, acid anhydrides is selectively 89.6%, and methyl acetate conversion ratio is 65%, carbonylation product acid
Acid anhydride yield is 85%.
(02) mean value of the continuous experimental data for repeating test three times of comparative example is as follows:
Carbonylation product is calculated by CO, and acid anhydrides is selectively that 93.9%, CO conversion ratio is 95.6%, and carbonyl products acid anhydrides is received
Rate is 91.3%, is calculated by methanol, acid anhydrides is selectively 89.5%, methanol conversion 92.5%, carbonylation product acid anhydrides yield
It is 90.3%, is calculated by methyl acetate, acid anhydrides is selectively 87.6%, and methyl acetate conversion ratio is 60.7%, carbonylation product
Acid anhydrides yield is 83%.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (5)
1. a kind of acetic acid aceticanhydride Joint Production and separation method characterized by comprising
S1, methanol and acetic acid the atmospheric synthesis methyl acetate under sulfuric acid catalyst effect, reaction temperature are 65-85 DEG C；
S2, methyl acetate, methanol are added reaction kettle, and are passed through CO, under the action of potassium iodide and rhodium series catalysts, in reaction pressure
Power 2.5-3Mpa under conditions of reaction temperature is 130-140 DEG C, carries out reaction and generates aceticanhydride, co-production acetic acid, by separating
To aceticanhydride and acetic acid.
2. acetic acid aceticanhydride Joint Production as described in claim 1 and separation method, which is characterized in that the reaction kettle includes:
Supporting table is horizontally placed on ground；
Door shaped stent, both ends are fixed on the supporting table；
Autoclave body is arranged below door shaped stent, and the autoclave body includes upper kettle and lower kettle；The lower kettle is no-top plate
Cylindrical housings shape, the inner cavity of the lower kettle have circular first for accommodating reaction solution, the side wall of the lower kettle
Interior hollow structure is used to accommodate recirculated water, in described first hollow structure by the side wall of the lower kettle be divided by it is interior extremely
Outer inner sidewall and lateral wall, be provided on the lateral wall of the lower kettle with described first in hollow structure perforation water outlet
And water inlet；The upper kettle is cylindrical housings shape cooperate with the inner cavity of the lower kettle, without bottom plate, the upper kettle
The seamless inner cavity for being sheathed on the lower kettle top in lower part；
A pair of first electric telescopic rod, non-telescoping end are fixed on the lateral part of the door shaped stent, and described first electronic stretches
The lower end of contracting bar straight down and is fixedly connected with the top plate of the upper kettle；
Ring flat-plate is arranged and is fixed on the top of the outer wall of the upper kettle；
Cylinder is scraped, is tubular, and is arranged and is fixed on outside the ring flat-plate；Hold level with both hands under the lower end for scraping cylinder and the lower kettle
Together, and stretch to it is described under attached body first in hollow structure, it is described scrape cylinder protrude into the lower part of hollow structure in first
Side wall is bonded the inside and outside side wall of the lower kettle；
Agitating device comprising the second electric telescopic rod, non-telescoping lower end are fixed on table on the bottom plate of the lower kettle vertically
The center in face, the non-telescoping lower end of the second electric telescopic rod is fixed with a pair of opposite and horizontally disposed first agitating paddle, described
Relatively fixed the second agitating paddle for having a pair of of level in the flexible end face of second electric telescopic rod.
3. acetic acid aceticanhydride Joint Production as claimed in claim 2 and separation method, which is characterized in that the reaction kettle further includes
Gas whirl spraying device comprising:
Third electric telescopic rod, non-telescoping upper end are fixed on the center of the top plate of the upper kettle, the third electric expansion
The end face vertical of the telescopic end of bar is downward and the upper end of a coaxially connected vertical bar, the outer cover of the vertical bar are equipped with an at least axis
It holds, the inner ring of bearing is fixed with the vertical bar, and the outside of the bearing is arranged and is fixed with the loop bar of a tubular, and external is spiral shell
Rotation stirring is rodlike；
Interfere mixing part, is set in the outside of the lower end of the loop bar, the interference mixing part is fixed on institute by a cross bar
On the inner wall for stating the lower part of upper kettle；
The lower end surface of the loop bar is coaxially fixed with a disk-shaped gas chamber, is the closed shell with cylindrical lumens
Shape, the bottom plate of the gas chamber invaginate to form multiple stomatas communicated with its inner cavity；
Soft tracheae, one end protrude into the inner cavity of the autoclave body, and are connected to the inner cavity of the gas chamber；
Wherein, when the third electric telescopic rod is flexible, the vertical bar can be driven to move downward or upward, the loop bar is in institute
State interference mixing part interference under can circumference forward or reverse.
4. acetic acid aceticanhydride Joint Production as claimed in claim 3 and separation method, which is characterized in that the bearing is a pair,
A pair of bearings is respectively sleeved at the upper and lower end of the vertical bar.
5. acetic acid aceticanhydride Joint Production as claimed in claim 3 and separation method, which is characterized in that multiple stomatas are uniformly distributed
On the bottom plate of the gas chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811509405.2A CN109627158B (en) | 2018-12-11 | 2018-12-11 | Acetic anhydride joint production and separation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811509405.2A CN109627158B (en) | 2018-12-11 | 2018-12-11 | Acetic anhydride joint production and separation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109627158A true CN109627158A (en) | 2019-04-16 |
| CN109627158B CN109627158B (en) | 2021-08-13 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117054617A (en) * | 2023-10-12 | 2023-11-14 | 西南石油大学 | High-temperature high-pressure acid rock reaction rate measuring device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117054617A (en) * | 2023-10-12 | 2023-11-14 | 西南石油大学 | High-temperature high-pressure acid rock reaction rate measuring device |
| CN117054617B (en) * | 2023-10-12 | 2023-12-12 | 西南石油大学 | High-temperature high-pressure acid rock reaction rate measuring device |
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| CN109627158B (en) | 2021-08-13 |
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