CN114315569A - Process for co-producing isopropanol and methyl acetate and production equipment thereof - Google Patents
Process for co-producing isopropanol and methyl acetate and production equipment thereof Download PDFInfo
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Abstract
The invention discloses a process for co-producing isopropanol and methyl acetate and production equipment thereof, belonging to the field of chemical production; the production method comprises the steps of carrying out gas phase extraction on a mixture of isopropanol and methanol obtained by the ester exchange reaction of isopropyl acetate and methanol, and purifying the isopropanol; the isopropyl acetate and methanol are subjected to transesterification reaction to obtain methyl acetate and methanol, the methyl acetate and the methanol pass through a condenser and then enter a high-pressure tower, and the high-purity methyl acetate is obtained; the electronic grade isopropanol and the superior grade methyl acetate can be finally obtained through ester exchange reaction, and the main product and the side products have high purity, high molecular utilization degree and excellent economic effect.
Description
Technical Field
The invention belongs to the field of chemical production, and relates to a process for co-producing isopropanol and methyl acetate and production equipment thereof.
Background
The isopropanol is a chemical product with great industrial application value, and is widely applied to a plurality of fields such as printing ink, coating, medical intermediate and the like. In recent years, global high-purity isopropanol realizes rapid development in the field of electronic industry cleaning agents, and the isopropanol just starts in the field in China, so that the market development space and opportunity are considerable; meanwhile, methyl acetate is mainly used as an organic solvent for various products such as paint, adhesive and the like and for producing acetic anhydride at present, or is directly used as an intermediate for producing medicines and pesticides, so that the application is extremely wide, and the market usage amount is enlarged year by year. The processes for producing isopropanol on the market today mainly comprise: (1) an indirect hydration method of propylene. Dissolving propylene in sulfuric acid aqueous solution or concentrated sulfuric acid, producing intermediate products of isopropyl bisulfate and diisopropyl sulfate through esterification reaction, and hydrolyzing the intermediate products of isopropyl bisulfate and diisopropyl sulfate to generate isopropanol; (2) the direct water-mixing method is characterized in that propylene directly undergoes hydration reaction under the action of a catalyst to generate isopropanol, and byproducts of n-propanol, isopropyl ether, acetone and the like can be divided into 3 types of gas-phase direct hydration method, liquid-phase direct hydration method and gas-liquid mixed phase method; (3) an acetone hydrogenation method, wherein copper or zinc oxide is adopted as a carrier catalyst or a nickel-based catalyst in the acetone hydrogenation method, and the acetone is hydrogenated to generate isopropanol at the temperature of 70-200 ℃ and under the normal pressure; (4) the acetic acid hydrogenation method, namely the acetic acid is hydrogenated to synthesize the isopropanol in one step, has short process flow, lower cost for producing the isopropanol and mild reaction conditions. These older processes result in lower yields of isopropyl alcohol, which is a gap from green manufacturing standards.
The method for producing the isopropanol by the ester exchange method has the advantages of mild reaction conditions (normal pressure), environmental protection, high raw material conversion rate, easy product separation and simple process flow. With the improvement of the environmental protection requirement of chemical production in recent years, the ester exchange method for producing the isopropanol has good development prospect.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a process for co-producing isopropanol and methyl acetate and production equipment thereof, and solves the problem of low conversion rate of isopropanol production in the prior art.
The purpose of the disclosure can be realized by the following technical scheme:
a production method for the coproduction of isopropanol and methyl acetate is characterized in that isopropanol and methanol mixture obtained by the ester exchange reaction of isopropyl acetate and methanol are extracted in a gas phase and then purified; and the isopropyl acetate and the methanol are subjected to transesterification reaction to obtain methyl acetate and methanol, the methyl acetate and the methanol enter a high-pressure tower through a condenser, and then the methyl acetate with high purity is obtained.
Further, the production method comprises the following devices: the device comprises an ester exchange reaction rectifying tower, an ester exchange reaction rectifying bulkhead tower, a high-pressure tower, a low-pressure tower, a tower 1 condenser, a tower 2 condenser, a tower 4 condenser, a tower 1 reboiler, a tower 4 reboiler, a heat exchanger, a gas compressor, a heat exchanger, a separator and a heat exchanger.
Further, the specific process route of the production method is as follows:
(1) the isopropyl acetate and the methanol enter a transesterification rectifying tower to carry out transesterification, the generated azeotropic mixture of the methyl acetate and the methanol partially returns to the tower after flowing through a condenser, and the other part enters a high-pressure tower;
(2) the isopropanol and methanol mixture obtained from the side of the ester exchange reaction rectifying tower is extracted in a gas phase and enters an ester exchange reaction rectifying bulkhead tower without a reboiler;
(3) high-purity methanol obtained at the top of the ester exchange reaction rectifying bulkhead tower flows through a condenser, and then part of the high-purity methanol returns to the tower, and part of the high-purity methanol is circularly pumped back to the ester exchange reaction rectifying tower to continuously participate in the reaction;
(4) part of the bottom of the ester exchange reaction rectifying tower enters a reboiler, and the other part of the bottom flows through a heat exchanger to obtain an isopropanol product with the purity of over 99.9 percent;
(5) a part of methyl acetate is extracted from the bottom of the high-pressure tower and flows through a heat exchanger, a high-pressure azeotropic mixture obtained from the top of the high-pressure tower flows through a gas compressor, the heat exchanger and a separator and enters a low-pressure tower for further purification;
(6) the high-purity methyl acetate is extracted from the high-pressure tower and flows through the heat exchanger to obtain the methyl acetate with the purity of more than 99.9 percent;
(7) all methyl acetate and low-concentration methanol entering the low-pressure tower are extracted from the top of the low-pressure tower in the form of low-pressure azeotrope, and a part of methyl acetate and low-concentration methanol flow through the 4-tower condenser and then return to the tower, and a part of methyl acetate and low-concentration methanol flow circularly pressurized and returned to the high-pressure tower by a pump and are mixed with the feed.
(8) And (3) allowing high-purity methanol obtained at the bottom of the low-pressure tower to flow through a 4-tower reboiler, returning a part of the high-purity methanol to the tower, allowing a part of the high-purity methanol to enter a heat exchanger, and pumping the part of the high-purity methanol to the ester exchange reaction rectifying tower by using a pump for cyclic pressurization to form circulation.
Furthermore, the dividing wall column reactive distillation device consists of 1 ester exchange reactive distillation column and 1 ester exchange reactive distillation dividing wall column without a reboiler.
Further, the number of the plates of the ester exchange reaction rectifying tower is 30, the operating pressure is 68-72 KPa, the temperature of the top of the tower is 40-50 ℃, and the temperature of the bottom of the tower is 75-85 ℃.
Further, the number of tower plates of the ester exchange reaction rectifying bulkhead tower is 6, the operating pressure is 78-84 KPa, the tower top temperature is 70-80 ℃, and the tower kettle temperature is 75-85 ℃.
Furthermore, the pressure swing rectification technology consists of a high-pressure tower and a low-pressure tower.
Furthermore, the variable-pressure rectification technology uses a heat pump rectification energy-saving technology.
Further, the operating pressure of the high-pressure tower is 900-910 KPa.
Further, the tower top temperature of the low-pressure tower is 32-36 ℃, and the tower kettle temperature is 50-60 ℃.
The beneficial effect of this disclosure:
1. according to the invention, the partition wall tower reaction rectification process and the pressure swing rectification process are combined, the electronic grade isopropanol and the superior grade methyl acetate can be finally obtained through the ester exchange reaction, the purity of the main product and the byproduct is high, the molecular utilization rate is high, and the economic effect is excellent;
2. on the premise of meeting the product separation requirement, the method of the invention not only can save the operation and equipment cost, simplify the process flow and greatly reduce the energy consumption of the whole flow by utilizing the dividing wall tower reaction rectification process;
3. the invention can effectively separate the azeotropic system of methyl acetate and methanol sensitive to pressure change by utilizing the pressure-swing rectification process, and the larger temperature difference between the high-pressure rectification tower and the low-pressure rectification tower can be fully utilized, thereby greatly reducing the energy consumption of the system by the heat integration process.
4. The whole process of the invention has no waste gas and waste liquid, the excessive methanol is recycled, the hundred percent utilization of the raw materials is realized, and the whole process flow is green and environment-friendly.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present disclosure, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of an embodiment of the disclosure.
Detailed Description
The technical solutions in the embodiments of the present disclosure will be clearly and completely described below with reference to the drawings in the embodiments of the present disclosure, and it is obvious that the described embodiments are only a part of the embodiments of the present disclosure, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
As shown in figure 1, the production equipment for co-production of isopropanol and methyl acetate comprises an ester exchange reaction rectifying tower (1), an ester exchange reaction rectifying bulkhead tower (2), a high-pressure tower (3), a low-pressure tower (4), a tower 1 condenser (5), a tower 2 condenser (6), a tower 4 condenser (7), a tower 1 reboiler (8), a tower 4 reboiler (9), a heat exchanger (10), a gas compressor (11), a heat exchanger (12), a separator (13) and a heat exchanger (14).
Example 1:
using the plant scheme shown in fig. 1, the starting materials were 99.9 wt% methanol and 99.9 wt% isopropyl acetate, with the following feed conditions: methanol 2150kg/h, 25 ℃, 101 kPa; 6845kg/h of isopropyl acetate, 25 ℃ and 101 kPa. The obtained product enters an ester exchange reaction rectifying tower (1) to carry out ester exchange reaction, the generated azeotropic mixture of methyl acetate and methanol flows through a condenser (5), part of the azeotropic mixture returns to the tower, and part of the azeotropic mixture enters a high-pressure tower (3); the mixture of isopropanol and methanol obtained from the side of the ester exchange reaction rectifying tower (1) is extracted in a gas phase and enters an ester exchange reaction rectifying bulkhead tower (2) without a reboiler; high-purity methanol obtained at the top of the ester exchange reaction rectifying bulkhead tower (2) flows through a condenser (6), part of the high-purity methanol returns to the tower, and part of the high-purity methanol circularly returns to the ester exchange reaction rectifying tower (1) to continuously participate in the reaction; part of the bottom of the tower 1 enters a reboiler (8), and part of the bottom of the tower flows through a heat exchanger (10) to obtain an isopropanol product with the purity of 99.91 WT% and the flow rate of 4030 kg/h; a part of methyl acetate is extracted from the bottom of the high-pressure tower (3) and flows through a heat exchanger (12), a high-pressure azeotropic mixture obtained from the top of the high-pressure tower (3) flows through a gas compressor (11), the heat exchanger (12) and a separator (13) and enters a low-pressure tower (4) for further purification; high-purity methyl acetate is extracted from the high-pressure tower (3) and flows through a heat exchanger (14) to obtain methyl acetate with the purity of 99.92 percent and the flow rate of 5000 kg/h; all methyl acetate and low-concentration methanol entering the low-pressure tower (4) are extracted from the top of the low-pressure tower (4) in the form of low-pressure azeotrope, a part of methyl acetate and low-concentration methanol flow through a 4-tower condenser (7) and return to the tower, and a part of methyl acetate and low-concentration methanol flow circularly pressurized by a pump and return to the high-pressure tower (3) to be mixed with the feed. High-purity methanol obtained at the bottom of the low-pressure tower (4) flows through a 4-tower reboiler (9), part of the high-purity methanol returns to the tower, and part of the high-purity methanol enters a heat exchanger (14) and is pumped back to the ester exchange reaction rectifying tower (1) by circulating pressurization of a pump to form circulation.
Isopropyl acetate and methanol are fed, and the theoretical plate numbers of 1, 2, 3 and 4 are respectively as follows: 30. 6, 30 and 30, operating pressures of 72kPa68, 84kPa, 910kPa and 50kPa, respectively. The used filler is a composite micropore type valve high-efficiency column plate filler.
According to analysis calculation, the energy consumption of a conventional device under the feed composition is about 5058.24kw, and the energy consumption is converted into standard coal:
and the heat pump technical device carries out heat exchange treatment between streams, so that energy consumption can be saved, the energy consumption is about 3979.53kw, and the standard coal is converted into the following components:
energy consumption is reduced:
example 2:
the apparatus flow shown in the attached figure 1 is adopted, raw materials are 99.8 wt% of methanol and 99.9 wt% of isopropyl acetate, and the feeding conditions are as follows: 2200kg/h of methanol, 25 ℃ and 101 kPa; 6900kg/h isopropyl acetate, 25 deg.C, 101 kPa. The obtained product enters an ester exchange reaction rectifying tower (1) to carry out ester exchange reaction, the generated azeotropic mixture of methyl acetate and methanol flows through a condenser (5), part of the azeotropic mixture returns to the tower, and part of the azeotropic mixture enters a high-pressure tower (3); the mixture of isopropanol and methanol obtained from the side of the ester exchange reaction rectifying tower (1) is extracted in a gas phase and enters an ester exchange reaction rectifying bulkhead tower (2) without a reboiler; high-purity methanol obtained at the top of the ester exchange reaction rectifying bulkhead tower (2) flows through a condenser (6), part of the high-purity methanol returns to the tower, and part of the high-purity methanol circularly returns to the ester exchange reaction rectifying tower (1) to continuously participate in the reaction; 1, part of the tower kettle enters a reboiler (8), and the other part of the tower kettle flows through a heat exchanger (10) to obtain an isopropanol product with the purity of 99.85 WT% and the flow rate of 3950 kg/h; a part of methyl acetate is extracted from the bottom of the high-pressure tower (3) and flows through a heat exchanger (12), a high-pressure azeotropic mixture obtained from the top of the high-pressure tower (3) flows through a gas compressor (11), the heat exchanger (12) and a separator (13) and enters a low-pressure tower (4) for further purification; high-purity methyl acetate is extracted from the high-pressure tower (3) and flows through a heat exchanger (14) to obtain methyl acetate with the purity of 99.87 percent and the flow rate of 4890 kg/h; all methyl acetate and low-concentration methanol entering the low-pressure tower (4) are extracted from the top of the low-pressure tower (4) in the form of low-pressure azeotrope, a part of methyl acetate and low-concentration methanol flow through a 4-tower condenser (7) and return to the tower, and a part of methyl acetate and low-concentration methanol flow circularly pressurized by a pump and return to the high-pressure tower (3) to be mixed with the feed. High-purity methanol obtained at the bottom of the low-pressure tower (4) flows through a 4-tower reboiler (9), part of the high-purity methanol returns to the tower, and part of the high-purity methanol enters a heat exchanger (14) and is pumped back to the ester exchange reaction rectifying tower (1) by circulating pressurization of a pump to form circulation.
Isopropyl acetate and methanol are fed, and the theoretical plate numbers of 1, 2, 3 and 4 are respectively as follows: 28. 8, 28 and 27 at operating pressures of 68kPa, 78kPa, 900kPa and 48kPa, respectively. The used filler is a composite micropore type valve high-efficiency column plate filler.
According to analysis calculation, the energy consumption of a conventional device under the feed composition is about 4955.84kw, and the energy consumption is converted into standard coal:
and the heat pump technical device carries out heat exchange treatment between streams, so that energy consumption can be saved, the energy consumption is about 3758.68kw, and the standard coal is converted into the following components:
energy consumption is reduced:
the embodiment can be used for reducing the energy consumption of the whole isopropanol production process.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (10)
1. A production method for coproducing isopropanol and methyl acetate is characterized in that the production method is used for extracting and purifying isopropanol in a gas phase from a mixture of isopropanol and methanol obtained by transesterification of isopropyl acetate and methanol; and the isopropyl acetate and the methanol are subjected to transesterification reaction to obtain methyl acetate and methanol, the methyl acetate and the methanol enter a high-pressure tower through a condenser, and then the methyl acetate with high purity is obtained.
2. The production method for the co-production of isopropanol and methyl acetate as claimed in claim 1, characterized in that the production method comprises the following devices: the device comprises an ester exchange reaction rectifying tower, an ester exchange reaction rectifying bulkhead tower, a high-pressure tower, a low-pressure tower, a tower 1 condenser, a tower 2 condenser, a tower 4 condenser, a tower 1 reboiler, a tower 4 reboiler, a heat exchanger, a gas compressor, a heat exchanger, a separator and a heat exchanger.
3. A process route for co-production of isopropanol and methyl acetate is characterized by comprising the following specific steps:
(1) the isopropyl acetate and the methanol enter a transesterification rectifying tower to carry out transesterification, the generated azeotropic mixture of the methyl acetate and the methanol partially returns to the tower after flowing through a condenser, and the other part enters a high-pressure tower;
(2) the isopropanol and methanol mixture obtained from the side of the ester exchange reaction rectifying tower is extracted in a gas phase and enters an ester exchange reaction rectifying bulkhead tower without a reboiler;
(3) high-purity methanol obtained at the top of the ester exchange reaction rectifying bulkhead tower flows through a condenser, and then part of the high-purity methanol returns to the tower, and part of the high-purity methanol is circularly pumped back to the ester exchange reaction rectifying tower to continuously participate in the reaction;
(4) part of the bottom of the ester exchange reaction rectifying tower enters a reboiler, and the other part of the bottom flows through a heat exchanger to obtain an isopropanol product with the purity of over 99.9 percent;
(5) a part of methyl acetate is extracted from the bottom of the high-pressure tower and flows through a heat exchanger, a high-pressure azeotropic mixture obtained from the top of the high-pressure tower flows through a gas compressor, the heat exchanger and a separator and enters a low-pressure tower for further purification;
(6) the high-purity methyl acetate is extracted from the high-pressure tower and flows through the heat exchanger to obtain the methyl acetate with the purity of more than 99.9 percent;
(7) all methyl acetate and low-concentration methanol entering the low-pressure tower are extracted from the top of the low-pressure tower in the form of low-pressure azeotrope, and a part of methyl acetate and low-concentration methanol flow through the 4-tower condenser and then return to the tower, and a part of methyl acetate and low-concentration methanol flow circularly pressurized and returned to the high-pressure tower by a pump and are mixed with the feed.
(8) And (3) allowing high-purity methanol obtained at the bottom of the low-pressure tower to flow through a 4-tower reboiler, returning a part of the high-purity methanol to the tower, allowing a part of the high-purity methanol to enter a heat exchanger, and pumping the part of the high-purity methanol to the ester exchange reaction rectifying tower by using a pump for cyclic pressurization to form circulation.
4. The dividing wall column reactive distillation apparatus of claim 3, wherein said apparatus comprises 1 transesterification reactive distillation column and 1 reboiler-free transesterification reactive distillation dividing wall column.
5. The process route of claim 3, wherein the number of the plates of the rectification column for the transesterification reaction is 30, the operating pressure is 68-72 KPa, the temperature at the top of the column is 40-50 ℃, and the temperature at the bottom of the column is 75-85 ℃.
6. The process route of claim 3, wherein the number of plates of the ester exchange reaction rectifying dividing wall column is 6, the operation pressure is 78-84 KPa, the temperature of the top of the column is 70-80 ℃, and the temperature of the bottom of the column is 75-85 ℃.
7. The pressure swing distillation technology included in the process route of claim 3, characterized by consisting of one higher pressure column and one lower pressure column.
8. The pressure swing rectification technology included in the process route according to claim 3 is characterized in that a heat pump rectification energy-saving technology is used.
9. The process route of claim 3, wherein the high pressure column operating pressure is 900 to 910 KPa.
10. The process route of claim 3, wherein the low-pressure column has a top temperature of 32 to 36 ℃ and a bottom temperature of 50 to 60 ℃.
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Cited By (2)
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| CN115232006A (en) * | 2022-06-17 | 2022-10-25 | 天津大学 | Method and device for producing isopropanol and co-producing methyl acetate by two-tower reaction-variable pressure mixed rectification and application |
| CN115253337A (en) * | 2022-06-17 | 2022-11-01 | 天津大学 | Method and device for preparing isopropanol through two-tower thermal coupling reaction-variable pressure mixed rectification and application |
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| CN103265429A (en) * | 2013-05-24 | 2013-08-28 | 青岛理工大学 | Technical method for synthesizing methyl acetate |
| CN109369340A (en) * | 2018-11-14 | 2019-02-22 | 常州大学 | A kind of device and method of reactive distillation transesterification preparing isopropanol |
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| CN115253337A (en) * | 2022-06-17 | 2022-11-01 | 天津大学 | Method and device for preparing isopropanol through two-tower thermal coupling reaction-variable pressure mixed rectification and application |
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