CN115232006A - Method and device for producing isopropanol and co-producing methyl acetate by two-tower reaction-variable pressure mixed rectification and application - Google Patents
Method and device for producing isopropanol and co-producing methyl acetate by two-tower reaction-variable pressure mixed rectification and application Download PDFInfo
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- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
- C07C29/1285—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis of esters of organic acids
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention discloses a device for producing isopropanol and co-producing methyl acetate by two-tower reaction-pressure swing mixed rectification, which comprises a reaction rectifying tower, a high-pressure rectifying tower, a first reboiler, a second reboiler, a first condenser, a second condenser, an auxiliary condenser, a first reflux tank, a second reflux tank and a mixer, wherein the reaction rectifying tower and the high-pressure rectifying tower are arranged along the vertical direction, and the upper part of the reaction rectifying tower is connected with the upper part in the high-pressure rectifying tower. The invention adopts the equal molar ratio reaction of isopropyl acetate and methanol, and avoids the problem of high energy consumption caused by large flow of methanol recovery cycle substances due to excessive methanol. The invention realizes the production of high-purity isopropanol and coproduces high-purity methyl acetate.
Description
Technical Field
The invention belongs to the technical field of separation and rectification, relates to a multi-component azeotrope separation technology and a reaction rectification and pressure swing rectification technology, and particularly relates to a method, a device and an application for producing isopropanol and co-producing methyl acetate by two-tower reaction-pressure swing mixed rectification.
Background
Isopropyl alcohol (IPA), which is called IPA for short, is a very important chemical product and raw material, and is commonly used as a disinfectant and preservative because of its excellent disinfecting and sterilizing effects. In recent years, the demand of disinfectants is increased in a global normalized situation of new crown blight, so that the demand of isopropanol is increased day by day. The traditional method for producing isopropanol comprises direct hydration and indirect hydration of propylene, namely propylene directly or indirectly reacts with water under the action of a catalyst to generate the isopropanol as the name suggests. The indirect hydration method is also called propene sulfuric acid hydration method, but the method has serious equipment corrosion caused by large consumption of catalyst sulfuric acid, low product selectivity and high energy consumption, and the method is gradually eliminated in China. The current commercial production of isopropanol is a direct hydration method, but the method adopts a gas or liquid phase direct hydration method or a gas-liquid mixed phase hydration method, so that the single-pass conversion rate of propylene is low, or the reaction condition is harsh, the requirement on the purity of raw materials is high, and the catalyst is expensive. In fact, one method for producing isopropanol is the acetone hydrogenation method, but the raw material acetone used in the method is high in cost, and the yield of the process is generally lower than that of the direct hydration method. Therefore, it is very important to find a more efficient, green and compact method for producing isopropanol.
Methyl acetate (Methyl acetate), also known as Methyl acetate, is an important basic organic chemical raw material, is used as an organic pollutant which is not limited to be used for emission, can reach the environmental protection standard, gradually replaces solvents such as acetone, butanone, ethyl acetate, cyclopentane and the like, is a green environment-friendly fast-drying solvent and an important chemical raw material, and is widely applied to the fields of coatings, printing ink, automobile industry, spices, foaming agents, polymer solvents, adhesives, medicinal chemicals and the like.
Chinese patent publication CN201210261305.9 provides a continuous reaction rectification process for synthesizing isopropanol and rectification equipment thereof, the method adopts homogeneous basic catalyst sodium methoxide, and although the product isopropanol with the mass fraction of more than 99% is obtained, the participation of the homogeneous catalyst makes the preparation process complicated due to the need of separating the homogeneous catalyst, thereby greatly increasing the process cost and energy consumption.
Chinese patent publication CN201210349759.1 provides a catalytic rectification process for synthesizing isopropanol by ester exchange method and a production apparatus thereof, the method uses heterogeneous cation exchange resin as a catalyst, which avoids the recovery of alkali salt catalyst, but in order to obtain isopropanol product with mass fraction greater than 99%, the method still needs four rectification towers to complete the production of isopropanol, and the process is still complicated.
Chinese patent publication CN107501042B provides a method for preparing isopropanol by hydrolyzing isopropyl acetate, which, despite the simple process, involves water to make the system heterogeneous, and presents a ternary azeotrope of isopropanol-water-isopropyl acetate. As is well known, the azeotrope-containing system has great separation difficulty, so that the separation difficulty and the separation cost are greatly increased, the purity of the isopropanol is greatly reduced, and only the isopropanol with the purity of 99 percent can be obtained.
By contrast, the present patent application is intrinsically different from the above patent publications.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method, a device and application for producing isopropanol and co-producing methyl acetate by two-tower reaction-pressure swing mixed rectification.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a device for producing isopropanol and co-producing methyl acetate by two-tower reaction-pressure swing mixed rectification comprises a reaction rectifying tower, a high-pressure rectifying tower, a first reboiler, a second reboiler, a first condenser, a second condenser, an auxiliary condenser, a first reflux tank, a second reflux tank and a mixer, wherein the reaction rectifying tower and the high-pressure rectifying tower are arranged along the vertical direction, and the upper part of the reaction rectifying tower is connected with the upper part in the high-pressure rectifying tower;
the top of the reactive distillation column is connected with a reactive gas outlet, and the upper part of the reactive distillation column is connected with a feed inlet and a discharge outlet of the reactive distillation column; the bottom of the reaction rectifying tower is connected with a first reboiler, the bottom of the reaction rectifying tower is connected with a material outlet, an isopropyl acetate feed port and a methanol mixture feed port are arranged at the upper and lower intervals of the reaction rectifying tower between the top and the bottom of the reaction rectifying tower, the methanol mixture feed port is connected with the output end of a mixer through a pump, the input end of the mixer comprises a methanol input end and a high-pressure rectifying tower condensation material input end, the methanol input end can input methanol, and the high-pressure rectifying tower condensation material input end is connected with the high-pressure rectifying tower through an auxiliary condenser and a pipeline; the reaction gas outlet is connected with the material inlet and the material outlet of the reaction rectifying tower through a first condenser, a first reflux tank and a pump, and a pipeline between the pump and the material inlet and the material outlet of the reaction rectifying tower is also connected with the material inlet of the reaction rectifying tower;
the bottom of the high-pressure rectifying tower is connected with a second reboiler, the bottom of the high-pressure rectifying tower is connected with a material outlet, the top of the high-pressure rectifying tower is connected with a high-pressure gas outlet, and the upper part of the high-pressure rectifying tower is provided with a material feeding hole and a material discharging hole of the high-pressure rectifying tower; the high-pressure gas outlet is connected with the feed inlet and the discharge outlet of the high-pressure rectifying tower through a second condenser, a second reflux tank and a pump, and the pipeline between the pump and the feed inlet and the discharge outlet of the high-pressure rectifying tower is connected with the condensed material input end of the high-pressure rectifying tower through an auxiliary condenser.
The application of the device in the production of isopropanol and the coproduction of methyl acetate is disclosed.
The method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
(1) Raw material isopropyl acetate enters a reactive distillation tower through a pump, a pipeline and an isopropyl acetate feed inlet, simultaneously methanol input in a mixer and material flow from the top of a high-pressure distillation tower enter the reactive distillation tower through the pipeline and the methanol mixture feed inlet, and high-purity product isopropyl alcohol is obtained at the bottom of the tower after reaction; the mixture at the top of the reaction rectifying tower enters a high-pressure rectifying tower from a reaction gas outlet at the top of the reaction rectifying tower in a gas phase form through a pump and a pipeline;
(2) The mixture from the top of the reaction rectifying tower is used as a raw material to enter a high-pressure rectifying tower, a high-purity product methyl acetate is obtained at the bottom of the tower, one stream of the material is pumped out from the high-pressure rectifying tower and returns to the top of the reaction rectifying tower through a pressure reducing valve and a pipeline, mass transfer, heat transfer and reaction are continuously carried out in the tower, the mixture at the top of the high-pressure rectifying tower is conveyed into an auxiliary condenser through a pipeline from a material inlet and a material outlet of the high-pressure rectifying tower in a gas phase mode, and the condensed mixture enters a mixer to be mixed and then flows into the reaction rectifying tower to be subjected to circular reaction rectification.
Further, the specific steps are as follows:
the isopropyl acetate and methanol containing a circulating material flow enter a reaction rectifying tower, ester exchange reaction is carried out under the action of a reaction section catalyst of the reaction rectifying tower, a reaction rectifying tower bottom material is heated by a reboiler and then is vaporized and ascends along the tower body, mass and heat transfer is continuously carried out with descending liquid at the upper part, meanwhile, the reaction rate of the isopropyl acetate and the methanol is accelerated, the rectification promotion reaction is realized, and a high-purity product isopropanol is extracted from the bottom of the reaction rectifying tower; the overhead of the reactive distillation tower flows through a first condenser to be condensed and enters a first reflux tank, one part of liquid in the first reflux tank refluxes and returns to the reactive distillation tower, and the other part of liquid is conveyed to the high-pressure distillation tower through a pump and a pipeline for secondary distillation;
the heat exchange material flow at the bottom of the high-pressure rectifying tower and the descending liquid at the upper part continuously transfer mass and heat, the high-purity product methyl acetate is extracted from the bottom of the high-pressure rectifying tower, the superheated steam at the top of the tower partially flows back to the high-pressure rectifying tower through a condenser, the other part of the liquid is condensed through an auxiliary condenser through a pipeline and then is mixed in a mixer, and then the mixed liquid is circularly returned to the reaction rectifying tower to continuously carry out reactive rectification.
Further, feeding in a mode of taking isopropyl acetate and methanol as an equimolar ratio, wherein the operating pressure of the reactive distillation tower is 1atm, and the operating pressure of the high-pressure distillation tower is 3-9atm.
Furthermore, the theoretical plate number of the reactive distillation column is 47-50 plates, the isopropyl acetate feeding position is 17-21 plates, the feeding position of the mixture at the top of the methanol and reactive distillation column is 17-21 plates, the reaction section is 19-39 plates, the reflux ratio is 0.96-1.08, the theoretical plate number of the high-pressure distillation column is 9-16 plates, the mixture feeding position is 2-4 plates, and the reflux ratio is 0.01-0.055.
Further, the catalyst is macroporous strong-acid cation exchange resin or KRD001.
Furthermore, the molar purity of the isopropanol product produced by the method is more than 99.50%, the molar recovery rate of the isopropanol is more than 99.50%, the molar purity of the co-produced methyl acetate product is more than 99.50%, and the molar recovery rate of the methyl acetate is more than 99.50%.
The invention has the advantages and positive effects that:
1. the invention adopts the equal molar ratio reaction of isopropyl acetate and methanol, and avoids the problem of high energy consumption caused by large flow of methanol recovery cycle substances due to excessive methanol.
2. The invention realizes the production of high-purity isopropanol and coproduces high-purity methyl acetate.
3. The invention adopts a two-tower reaction-pressure swing mixed rectification method, obtains a high-purity product, and simultaneously has simple flow and convenient operation, and greatly reduces the cost problem caused by the complexity of the process.
4. The method not only efficiently produces the high-purity isopropanol, but also coproduces the methyl acetate, and only adopts one reaction rectifying tower and one variable-pressure tower rectifying tower, so that the reaction condition is mild, the process is simple, the operation is simple and convenient, and the production cost is greatly reduced.
5. The method takes isopropyl acetate and methanol as raw materials, and adopts two-tower reaction-pressure swing mixed rectification to obtain the product isopropanol with the molar purity of more than 99.50 percent, the molar recovery rate of the isopropanol of more than 99.50 percent, the molar purity of the co-production product methyl acetate of more than 99.50 percent, and the molar recovery rate of the methyl acetate of more than 99.50 percent.
6. The invention takes isopropyl acetate and methanol as raw materials, takes commercial macroporous strong-acid cation exchange resin as a catalyst, and adopts a process method of two-tower reaction-pressure swing mixed rectification to produce methyl acetate co-produced by isopropyl alcohol. The method not only successfully realizes the high-purity production of the isopropanol, but also co-produces the high-purity methyl acetate; the method adopts commercial macroporous strong-acid cation exchange resin as a catalyst, so that the problem of recovery of a homogeneous catalyst is avoided; the two-tower reaction-pressure swing mixed rectification process is simple in flow, the limitation of chemical balance is broken through the reactive rectification, and the energy consumption of the process is reduced.
7. The device of the invention adopts a normal-pressure reaction rectifying tower and a high-pressure rectifying tower, realizes the high-purity production of the isopropanol and produces the high-purity methyl acetate in parallel.
Drawings
FIG. 1 is a schematic diagram of a structural connection of a rectifying apparatus according to the present invention.
Detailed Description
The following detailed description of the embodiments of the present invention is provided for the purpose of illustration and not limitation, and should not be construed as limiting the scope of the invention.
The raw materials used in the invention are conventional commercial products unless otherwise specified; the methods used in the present invention are conventional in the art unless otherwise specified.
A device for producing isopropanol and co-producing methyl acetate by two-tower reaction-pressure swing mixed rectification is shown in figure 1 and comprises a reaction rectifying tower T1, a high-pressure rectifying tower T2, a first reboiler R1, a second reboiler R2, a first condenser C1, a second condenser C2, an auxiliary condenser H, a first reflux tank A1, a second reflux tank A2 and a mixer M, wherein the reaction rectifying tower and the high-pressure rectifying tower are arranged along the vertical direction, and the upper part of the reaction rectifying tower is connected with the upper part in the high-pressure rectifying tower;
the top of the reactive distillation column is connected with a reactive gas outlet 3, and the upper part of the reactive distillation column is connected with a feed inlet and a discharge outlet 4 of the reactive distillation column; the bottom of the reaction rectifying tower is connected with a first reboiler, the bottom of the reaction rectifying tower is connected with a material outlet (not numbered in the figure), the upper portion and the lower portion of the reaction rectifying tower between the top and the bottom of the reaction rectifying tower are provided with an isopropyl acetate feed port 1 and a methanol mixture feed port 2 at intervals, the methanol mixture feed port is connected with the output end of the mixer through a pump, the input end of the mixer comprises a methanol input end and a material condensation input end (not numbered in the figure) of the high-pressure rectifying tower, the methanol input end can input methanol, and the material condensation input end of the high-pressure rectifying tower is connected with the high-pressure rectifying tower through an auxiliary condenser and a pipeline; the reaction gas outlet is connected with the feed inlet and the discharge outlet of the reaction rectifying tower through a first condenser, a first reflux tank and a pump, and a pipeline between the pump and the feed inlet and the discharge outlet of the reaction rectifying tower is also connected with the feed inlet of the reaction rectifying tower;
the bottom of the high-pressure rectifying tower is connected with a second reboiler, the bottom of the high-pressure rectifying tower is connected with a material outlet (not numbered in the figure), the top of the high-pressure rectifying tower is connected with a high-pressure gas outlet 6, and the upper part of the high-pressure rectifying tower is provided with a material inlet 5 of the reactive rectifying tower and a material inlet and outlet 7 of the high-pressure rectifying tower; the high-pressure gas outlet is connected with the feed inlet and the discharge outlet of the high-pressure rectifying tower through a second condenser, a second reflux tank and a pump, and the pipeline between the pump and the feed inlet and the discharge outlet of the high-pressure rectifying tower is connected with the condensed material input end of the high-pressure rectifying tower through an auxiliary condenser.
The material outlet of the reactive distillation column can be connected with the product outlet material flow B1 to discharge related products, and the material outlet of the high-pressure distillation column can be connected with the product outlet material flow B2 to discharge related products.
The application of the device in the production of isopropanol and the coproduction of methyl acetate is disclosed.
The method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
(1) Raw material isopropyl acetate enters a reactive distillation tower through a pump, a pipeline and an isopropyl acetate feed inlet, methanol input in a mixer and material flow from the top of a high-pressure distillation tower enter the reactive distillation tower through the pipeline and a methanol mixture feed inlet, and high-purity product isopropyl alcohol is obtained at the bottom of the tower after reaction; the mixture at the top of the reaction rectifying tower enters a high-pressure rectifying tower from a reaction gas outlet at the top of the reaction rectifying tower in a gas phase form through a pump and a pipeline;
(2) The mixture from the top of the reaction rectifying tower is used as a raw material to enter a high-pressure rectifying tower, a high-purity product methyl acetate is obtained at the bottom of the tower, one stream of the material is pumped out from the high-pressure rectifying tower and returns to the top of the reaction rectifying tower through a pressure reducing valve and a pipeline, mass transfer, heat transfer and reaction are continuously carried out in the tower, the mixture at the top of the high-pressure rectifying tower is conveyed into an auxiliary condenser through a pipeline from a material inlet and a material outlet of the high-pressure rectifying tower in a gas phase mode, and the condensed mixture enters a mixer to be mixed and then flows into the reaction rectifying tower to be subjected to circular reaction rectification.
Further, the specific steps are as follows:
the isopropyl acetate and methanol containing a circulating material flow enter a reaction rectifying tower, ester exchange reaction is carried out under the action of a reaction section catalyst of the reaction rectifying tower, a reaction rectifying tower bottom is heated by a reboiler and then vaporized, the vaporization is carried out along a tower body, mass and heat transfer is continuously carried out with upper descending liquid, the reaction rate of the isopropyl acetate and the methanol is accelerated, the rectification promotion reaction is realized, and a high-purity product isopropanol is extracted from the bottom of the reaction rectifying tower; the overhead of the reactive distillation tower flows through a first condenser to be condensed and enters a first reflux tank, one part of liquid in the first reflux tank refluxes and returns to the reactive distillation tower, and the other part of liquid is conveyed to the high-pressure distillation tower through a pump and a pipeline for secondary distillation;
the heat exchange material flow at the bottom of the high-pressure rectifying tower and the descending liquid at the upper part continuously transfer mass and heat, the high-purity product methyl acetate is extracted from the bottom of the high-pressure rectifying tower, the superheated steam at the top of the tower partially flows back to the high-pressure rectifying tower through a condenser, the other part of the liquid is condensed through an auxiliary condenser through a pipeline and then is mixed in a mixer, and then the mixed liquid is circularly returned to the reaction rectifying tower to continuously carry out reactive rectification.
Preferably, the isopropyl acetate and the methanol are fed in an equimolar ratio, the operating pressure of the reactive distillation tower is 1atm, and the operating pressure of the high-pressure distillation tower is 3-9atm.
Preferably, the theoretical plate number of the reactive distillation column is 47-50 plates, the feeding position of isopropyl acetate is 17-21 plates, the feeding position of a mixture of methanol and the top of the reactive distillation column is 17-21 plates, the reaction section is 19-39 plates, the reflux ratio is 0.96-1.08, the theoretical plate number of the high-pressure distillation column is 9-16 plates, the feeding position of the mixture is 2-4 plates, and the reflux ratio is 0.01-0.055.
Preferably, the catalyst is a macroporous strong acid cation exchange resin or KRD001.
Preferably, the molar purity of the isopropanol product produced by the method is more than 99.50%, the molar recovery rate of the isopropanol is more than 99.50%, the molar purity of the co-produced methyl acetate product is more than 99.50%, and the molar recovery rate of the methyl acetate is more than 99.50%.
Specifically, the preparation and detection examples are as follows:
the following examples illustrate the need for 2800 tons of isopropyl alcohol produced annually in a chemical plant in south China (300 days a year, 24 hours a day).
Example 1:
the method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
the feeding temperature of the fresh raw materials is 45 ℃, the raw materials are fed according to the equal molar ratio, the flow rate of isopropyl acetate is 350kg/h, and the flow rate of methanol is 109.81kg/h. The theoretical plate number of the reactive distillation column (T1) is 48, the feeding plates of isopropyl acetate and methanol are 20, the reaction section is between 19 and 38 plates, the operating pressure is 1atm, the inner diameter of the column is 0.621m, and the reflux ratio is 1.08; the theoretical plate number of the high-pressure rectifying tower (T2) is 16, the feed plate is 4, the operating pressure is 3atm, the inner diameter of the tower is 0.411m, and the reflux ratio is 0.145. The molar purity of the obtained isopropanol product is 99.56 percent, the molar yield is 99.56 percent, and the molar purity of the coproduction product methyl acetate is 99.95 percent, and the yield is 99.56 percent.
Example 2:
the method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
the feeding temperature of the fresh raw materials is 45 ℃, the raw materials are fed according to the equal molar ratio, the flow rate of isopropyl acetate is 350kg/h, and the flow rate of methanol is 109.81kg/h. The theoretical plate number of the reactive distillation tower (T1) is 48, the isopropyl acetate and methanol feeding plates are 21, the reaction section is between 19 and 38 plates, the operating pressure is 1atm, the inner diameter of the tower is 0.603m, and the reflux ratio is 0.96; the theoretical plate number of the high-pressure rectifying tower (T2) is 12, the feeding plate is 2, the operating pressure is 4atm, the inner diameter of the tower is 0.386m, and the reflux ratio is 0.055. The molar purity of the obtained isopropanol product is 99.50%, the molar yield is 99.50%, and the molar purity of the co-produced methyl acetate product is 99.51%, and the yield is 99.51%.
Example 3:
the method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
the feeding temperature of the fresh raw materials is 45 ℃, the raw materials are fed according to the equal molar ratio, the flow rate of isopropyl acetate is 350kg/h, and the flow rate of methanol is 109.81kg/h. The theoretical plate number of the reactive distillation column (T1) is 50, the isopropyl acetate and methanol feeding plates are 21, the reaction section is between 19 and 39 plates, the operating pressure is 1atm, the inner diameter of the column is 0.596m, and the reflux ratio is 0.929; the theoretical plate number of the high-pressure rectifying tower (T2) is 11, the feeding plate is 2, the operation pressure is 5atm, the inner diameter of the tower is 0.375m, and the reflux ratio is 0.01. The molar purity of the obtained isopropanol product is 99.50%, the molar yield is 99.50%, and the molar purity of the co-produced methyl acetate product is 99.51%, and the yield is 99.51%.
Example 4:
the method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
the feeding temperature of fresh raw materials is 45 ℃, the raw materials are fed according to the equal molar ratio, the flow rate of isopropyl acetate is 350kg/h, and the flow rate of methanol is 109.81kg/h. The theoretical plate number of the reactive distillation tower (T1) is 47, the isopropyl acetate and methanol feeding plates are 17, the reaction section is between 25 and 39 plates, the operating pressure is 1atm, the inner diameter of the tower is 0.621m, and the reflux ratio is 0.991; the theoretical plate number of the high-pressure rectifying tower (T2) is 9, the feeding plate is 2, the operation pressure is 7atm, the inner diameter of the tower is 0.374m, and the reflux ratio is 0.05. The molar purity of the obtained isopropanol product is 99.51 percent, the molar yield is 99.51 percent, and the molar purity of the coproduction product methyl acetate is 99.50 percent, and the yield is 99.50 percent.
Example 5:
the method for producing isopropanol and coproducing methyl acetate by utilizing the two-tower reaction-pressure swing mixed rectification of the device comprises the following steps:
the feeding temperature of the fresh raw materials is 45 ℃, the raw materials are fed according to the equal molar ratio, the flow rate of isopropyl acetate is 350kg/h, and the flow rate of methanol is 109.81kg/h. The theoretical plate number of the reaction rectifying tower (T1) is 47, the isopropyl acetate and methanol feeding plates are 17, the reaction section is 25-39 plates, the operation pressure is 1atm, the inner diameter of the tower is 0.605m, and the reflux ratio is 0.983; the theoretical plate number of the high-pressure rectifying tower (T2) is 9, the feeding plate is 2, the operating pressure is 9atm, the inner diameter of the tower is 0.370m, and the reflux ratio is 0.02. The molar purity of the obtained isopropanol product is 99.51 percent, the molar yield is 99.51 percent, and the molar purity of the coproduction product methyl acetate is 99.51 percent, and the yield is 99.51 percent.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the embodiments disclosed.
Claims (8)
1. A device for producing isopropanol and co-producing methyl acetate by two-tower reaction-pressure swing mixed rectification is characterized in that: the device comprises a reaction rectifying tower, a high-pressure rectifying tower, a first reboiler, a second reboiler, a first condenser, a second condenser, an auxiliary condenser, a first reflux tank, a second reflux tank and a mixer, wherein the reaction rectifying tower and the high-pressure rectifying tower are arranged along the vertical direction, and the upper part of the reaction rectifying tower is connected with the upper part in the high-pressure rectifying tower;
the top of the reactive distillation column is connected with a reactive gas outlet, and the upper part of the reactive distillation column is connected with a feed inlet and a discharge outlet of the reactive distillation column; the bottom of the reaction rectifying tower is connected with a first reboiler, the bottom of the reaction rectifying tower is connected with a material outlet, an isopropyl acetate feed port and a methanol mixture feed port are arranged at the upper and lower intervals of the reaction rectifying tower between the top and the bottom of the reaction rectifying tower, the methanol mixture feed port is connected with the output end of a mixer through a pump, the input end of the mixer comprises a methanol input end and a high-pressure rectifying tower condensation material input end, the methanol input end can input methanol, and the high-pressure rectifying tower condensation material input end is connected with the high-pressure rectifying tower through an auxiliary condenser and a pipeline; the reaction gas outlet is connected with the feed inlet and the discharge outlet of the reaction rectifying tower through a first condenser, a first reflux tank and a pump, and a pipeline between the pump and the feed inlet and the discharge outlet of the reaction rectifying tower is also connected with the feed inlet of the reaction rectifying tower;
the bottom of the high-pressure rectifying tower is connected with a second reboiler, the bottom of the high-pressure rectifying tower is connected with a material outlet, the top of the high-pressure rectifying tower is connected with a high-pressure gas outlet, and the upper part of the high-pressure rectifying tower is provided with a material feeding hole and a material discharging hole of the high-pressure rectifying tower; the high-pressure gas outlet is connected with the feed inlet and the discharge outlet of the high-pressure rectifying tower through a second condenser, a second reflux tank and a pump, and the pipeline between the pump and the feed inlet and the discharge outlet of the high-pressure rectifying tower is connected with the condensed material input end of the high-pressure rectifying tower through an auxiliary condenser.
2. Use of the apparatus of claim 1 for the co-production of isopropyl alcohol and methyl acetate.
3. A method for producing isopropanol and co-producing methyl acetate by using two-tower reaction-pressure swing mixed rectification of the device as claimed in claim 1, which is characterized in that: the method comprises the following steps:
(1) Raw material isopropyl acetate enters a reactive distillation tower through a pump, a pipeline and an isopropyl acetate feed inlet, simultaneously methanol input in a mixer and material flow from the top of a high-pressure distillation tower enter the reactive distillation tower through the pipeline and the methanol mixture feed inlet, and high-purity product isopropyl alcohol is obtained at the bottom of the tower after reaction; the mixture at the top of the reaction rectifying tower enters a high-pressure rectifying tower from a reaction gas outlet at the top of the tower in a gas phase form through a pump and a pipeline;
(2) The mixture from the top of the reaction rectifying tower is used as a raw material to enter a high-pressure rectifying tower, a high-purity product methyl acetate is obtained at the bottom of the tower, one stream of the material is pumped out from the high-pressure rectifying tower and returns to the top of the reaction rectifying tower through a pressure reducing valve and a pipeline, mass transfer, heat transfer and reaction are continuously carried out in the tower, the mixture at the top of the high-pressure rectifying tower is conveyed into an auxiliary condenser through a pipeline from a material inlet and a material outlet of the high-pressure rectifying tower in a gas phase mode, and the condensed mixture enters a mixer to be mixed and then flows into the reaction rectifying tower to be subjected to circular reaction rectification.
4. The method of claim 3, wherein: the method comprises the following specific steps:
the isopropyl acetate and methanol containing a circulating material flow enter a reaction rectifying tower, ester exchange reaction is carried out under the action of a reaction section catalyst of the reaction rectifying tower, a reaction rectifying tower bottom material is heated by a reboiler and then is vaporized and ascends along the tower body, mass and heat transfer is continuously carried out with descending liquid at the upper part, meanwhile, the reaction rate of the isopropyl acetate and the methanol is accelerated, the rectification promotion reaction is realized, and a high-purity product isopropanol is extracted from the bottom of the reaction rectifying tower; the overhead of the reactive distillation tower flows through a first condenser to be condensed and enters a first reflux tank, one part of liquid in the first reflux tank refluxes and returns to the reactive distillation tower, and the other part of liquid is conveyed to the high-pressure distillation tower through a pump and a pipeline for secondary distillation;
the heat exchange material flow at the bottom of the high-pressure rectifying tower and the descending liquid at the upper part continuously transfer mass and heat, the high-purity product methyl acetate is extracted from the bottom of the high-pressure rectifying tower, the superheated steam at the top of the tower partially flows back to the high-pressure rectifying tower through a condenser, the other part of the liquid is condensed through an auxiliary condenser through a pipeline and then is mixed in a mixer, and then the mixed liquid is circularly returned to the reaction rectifying tower to continuously carry out reactive rectification.
5. The method of claim 3, wherein: feeding in a mode of taking isopropyl acetate and methanol as an equimolar ratio, wherein the operating pressure of the reactive distillation tower is 1atm, and the operating pressure of the high-pressure distillation tower is 3-9atm.
6. The method of claim 3, wherein: the theoretical plate number of the reactive distillation tower is 47-50 plates, the feeding position of isopropyl acetate is 17-21 plates, the feeding position of a mixture at the top of the methanol and reactive distillation tower is 17-21 plates, the reaction section is 19-39 plates, the reflux ratio is 0.96-1.08, the theoretical plate number of the high-pressure distillation tower is 9-16 plates, the feeding position of the mixture is 2-4 plates, and the reflux ratio is 0.01-0.055.
7. The method of claim 3, wherein: the catalyst is macroporous strong-acid cation exchange resin or KRD001.
8. The method according to any one of claims 3 to 7, wherein: the molar purity of the isopropanol product produced by the method is more than 99.50 percent, the molar recovery rate of the isopropanol product is more than 99.50 percent, the molar purity of the co-produced methyl acetate product is more than 99.50 percent, and the molar recovery rate of the methyl acetate product is more than 99.50 percent.
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