CN107573227B - Equipment and method for preparing isophorone by acetone gas phase condensation - Google Patents
Equipment and method for preparing isophorone by acetone gas phase condensation Download PDFInfo
- Publication number
- CN107573227B CN107573227B CN201710766032.6A CN201710766032A CN107573227B CN 107573227 B CN107573227 B CN 107573227B CN 201710766032 A CN201710766032 A CN 201710766032A CN 107573227 B CN107573227 B CN 107573227B
- Authority
- CN
- China
- Prior art keywords
- tower
- acetone
- partition
- isophorone
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention relates to equipment and a method for preparing isophorone by acetone gas phase condensation, wherein the equipment comprises the following steps: the device comprises an acetone recovery tower, a first partition tower, an mesityl oxide tower and a second partition tower; in the first partition wall tower, a partition plate is positioned on a central axis in the tower, an azeotropic distillation area is positioned on the left side of the partition plate, and a water purification area is positioned on the right side of the partition plate; in the second partition wall tower, the partition is positioned on a central axis in the tower, the primary distillation zone is positioned on the left side of the partition, the lateral line zone is positioned on the right side of the partition, the public distillation section is positioned on the upper part of the partition, and the public stripping section is positioned on the lower part of the partition. The invention adopts novel separation technologies such as a partition tower and the like, and can effectively separate and recover various products in the acetone condensation reaction: main products of isophorone, byproducts of mesitylene, tetramer and the like, and the mass purity of each product is more than or equal to 99.60 percent; in addition, the invention obviously simplifies the process flow of preparing isophorone by acetone condensation and reduces equipment investment and energy consumption.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to equipment and a method for preparing isophorone by acetone gas phase condensation.
Background
Isophorone is one of important products for acetone deep processing, and the application is very wide; the high boiling point solvent having excellent performance is a solvent which can dissolve nitrocellulose, acrylic resin, alkyd resin, polyvinyl acetate resin, epoxy resin, and the like, and is also an industrial raw material of polymer solid propellants such as plastics, adhesives, medicines, inks, and pesticides. Isophorone is widely used: isophorone diamine (IPDA) synthesized by the method can be used as an epoxy resin curing agent; the isophorone diisocyanate (IPDI) produced by the method can be used as a raw material of a high-grade paint, so that the service life of the paint can be prolonged, yellowing can not occur, and the IPDI can still have good performance when being used as an automobile paint for more than 5 years; the trimethyl adipic acid prepared by the method can be used for producing novel plasticizers, lubricants, dinitrile, diamine, diol and the like; the 3, 5-xylenol synthesized by the method can be used as an insecticide. In recent years, with the continuous expansion of the application field of isophorone and the continuous improvement of the requirement of the industry of environment-friendly coatings, the isophorone coating has wide market demand and application prospect.
The synthesis method of isophorone can be divided into the isopropylidene acetone method and the acetone condensation method. The isopropylidene acetone method is difficult to popularize and apply due to higher raw material price and high product cost, and is eliminated. The acetone condensation method is divided into a liquid phase condensation method and a gas phase condensation method, and the acetone liquid phase condensation method is mostly adopted in industrial production: the method has the problems of easy corrosion of equipment, difficult separation and recovery, low acetone conversion rate, high production cost and the like. The acetone gas-phase condensation method has the advantages of no pollution, convenient operation and the like, and is suitable for large-scale industrial production, but the key points of the method are to find a suitable catalyst and develop a process with low energy consumption.
Chinese patent CN1166481 discloses a method for preparing isophorone: acetone and a catalyst are heated together under a high-pressure state and react under the liquid phase or gas phase condition, the acetone conversion rate is 25 percent, the isophorone selectivity is 37 percent, but the method does not carry out the subsequent separation treatment of products.
CN101633610A discloses a method for preparing isophorone by a supercritical method, which comprises the steps of carrying out supercritical reaction on acetone and a catalyst solution in a tubular reactor with the pressure of 8.0-20 MPa and the temperature of 280-320 ℃, enabling a reaction solution to enter a flash tower after pressure reduction, obtaining unreacted acetone from the top of the tower, enabling a tower bottom solution to enter a hydrolysis tower to hydrolyze polymers in the acetone, wherein the reaction time required by synthesizing α -isophorone by the method is short, the number of byproducts is small, but the reaction is realized by utilizing the supercritical condition, the conditions are harsh, the equipment investment is large, the energy consumption is high, the reaction rate of side reaction can be accelerated at high temperature, and the control difficulty is large.
CN102633612A discloses a preparation method of isophorone: continuously feeding acetone into a first reaction tower to perform condensation reaction to generate diacetone alcohol mixed solution; enabling the diacetone alcohol mixed solution to flow out of the first reaction tower, then flowing into a heat exchanger through a feed pump, heating to generate a diacetone alcohol dehydration reaction, and generating a mixture of acetone and mesityl oxide; putting the mixture of acetone and mesityl oxide and the rest diacetone alcohol mixed solution and a catalyst into a second reaction tower for reaction, cooling the prepared reaction solution, and separating out a gas phase, an oil phase and a water phase, wherein the oil phase is isophorone synthetic solution; and neutralizing and rectifying the isophorone synthetic solution to obtain finished product isophorone. The method has 3 defects: firstly, diacetone alcohol mixed liquor reacts in a heat exchanger and is difficult to control; secondly, the catalyst KOH solution in the second reaction tower can corrode equipment; finally, the product obtained by the method is isophorone synthetic solution, and the isophorone product can be obtained only by subsequent neutralization and rectification treatment.
In summary, it is important to provide a novel method for preparing isophorone, so as to simplify the process flow and reduce the energy consumption of equipment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide equipment and a method for preparing isophorone by acetone gas phase condensation. The invention adopts novel separation technologies such as a partition tower and the like, and can effectively separate and recover various products in the acetone condensation reaction: main products of isophorone, byproducts of mesitylene, tetramer and the like, and the mass purity of each product is more than or equal to 99.60 percent; in addition, the invention obviously simplifies the process flow of preparing isophorone by acetone condensation and reduces equipment investment and energy consumption.
In a first aspect, the present invention provides an apparatus for preparing isophorone by vapor phase condensation of acetone, comprising: the device comprises an acetone recovery tower, a first partition tower, an mesityl oxide tower and a second partition tower; wherein, the middle part of the acetone recovery tower is provided with a first feed inlet, and the bottom of the tower is provided with a first discharge outlet; in the first partition wall tower, a partition plate is positioned on a central axis in the tower, an azeotropic distillation area is positioned on the left side of the partition plate, a water purification area is positioned on the right side of the partition plate, a second feed inlet is arranged in the middle of the azeotropic distillation area, the second feed inlet is connected with a first discharge outlet through a pipeline, and a second discharge outlet is arranged at the bottom of the first partition wall tower; in the mesityl oxide tower, a third feed inlet is arranged in the middle of the mesityl oxide tower, the third feed inlet is connected with the second discharge outlet through a pipeline, and a third discharge outlet is arranged at the bottom of the mesityl oxide tower; in the second partition wall tower, the baffle is located the center axis in the tower, and the preliminary distillation district is located the baffle left side, and the siding district is located the baffle right side, and public rectification section is located baffle upper portion, and public stripping section is located the baffle lower part, and the middle part in preliminary distillation district is provided with the fourth feed inlet, and the fourth feed inlet passes through pipe connection with the third discharge gate, and the middle part in siding district is provided with the fourth discharge gate. Those skilled in the art will appreciate that: the dividing wall tower divides the tower into different areas by arranging a vertical dividing wall in the common rectifying tower, and the heat transfer is realized by utilizing vapor-liquid phase coupling material flow between the areas, so that the separation task which can be finished by two towers in the conventional rectifying process can be finished in one tower.
In a further embodiment of the present invention, one or more of a vaporizer, a heat exchanger, a condenser, a reboiler, and a liquid separation tank are further provided between the acetone recovery column, the first divided wall column, the mesityl oxide column, and the second divided wall column. Specifically, the vaporizer, the heat exchanger, the condenser, the reboiler, the liquid separation tank and the like can be specifically arranged by those skilled in the art according to actual conditions.
In a further embodiment of the present invention, the number of theoretical plates of the acetone recovery column is 40 to 65, and the number of theoretical plates of the mesityl oxide column is 25 to 50; in the first dividing wall tower, the theoretical plate number of the water purification area is 10-20, the theoretical plate number of the azeotropic rectification area is 30-50, and the first dividing wall tower is an azeotropic dividing wall tower; in the second dividing wall tower, the number of theoretical plates in the initial distillation zone is 10-25, the number of theoretical plates in the side line zone is 15-30, the number of theoretical plates in the public rectification section is 5-15, and the number of theoretical plates in the public stripping section is 4-25.
In a further embodiment of the present invention, in the second divided wall column, the withdrawal position of the fourth discharge port is the 5 th to 15 th trays in the side line region.
In a further embodiment of the present invention, the acetone recovery column, the first divided wall column, the mesityl oxide column and the second divided wall column are plate columns or packed columns.
In a second aspect, the present invention provides a method for preparing isophorone by acetone vapor phase condensation, which adopts the arrangement provided by the present invention, and comprises the following steps: s101: feeding the product of the acetone condensation reaction into an acetone recovery tower through a first feed inlet to recover acetone, then obtaining a first mixture at a first discharge outlet, obtaining high-purity acetone at the tower top, and then recycling the acetone to a vaporizer for reuse; s102: the first mixture enters a first bulkhead tower through a second feed inlet for dehydration treatment, and then a second mixture is obtained at a second discharge outlet; s103: feeding the second mixture into an mesityl oxide tower, and then obtaining a third mixture at a third discharge hole to obtain high-purity mesityl oxide at the tower top; s104: and (4) feeding the third mixture into a second partition tower, and then obtaining isophorone at a fourth discharge hole.
In a further embodiment of the present invention, step S100 is further included before S101: reacting raw material acetone in a fixed bed reactor under the action of a catalyst, and then exchanging heat between a product of the fixed bed reactor and the raw material acetone to obtain a product of acetone condensation reaction, wherein the product comprises a target product isophorone, byproducts of mesitylene, a tetramer and impurity water.
In a further embodiment of the invention, there is also included supplementing the first divided wall column with an azeotropic agent; the entrainer comprises one or more of n-propyl formate, n-butyl acetate, ethyl acetate and isobutyl formate.
In a further embodiment of the present invention, in S101, the top temperature of the acetone recovery column is 39 to 66 ℃, the bottom temperature of the acetone recovery column is 75 to 105 ℃, and the operating pressure is 0.5 to 2.5 atm; in S102, the operating pressure of a first partition wall tower is 0.5-2.5 atm, the temperature of the top of the tower is 50-80 ℃, and the temperature of the bottom of the tower is 70-105 ℃; in S103, the temperature of the top of the mesityl oxide tower is 40-69 ℃, the temperature of the bottom of the mesityl oxide tower is 120-165 ℃, and the operating pressure is 0.15-1.0 atm; in S104, the operating pressure of the second partition wall tower is 0.1-1.0 atm, the tower top temperature is 45-95 ℃, and the tower bottom temperature is 120-175 ℃.
The technical scheme provided by the invention has the following advantages:
(1) the applicant has found through a great deal of research that: by adopting the scheme provided by the invention, the products in the acetone condensation reaction can be effectively separated and recovered: main products of isophorone, byproducts of mesitylene, tetramer and the like, and the mass purity of each product is more than or equal to 99.60 percent; in other words, the scheme provided by the invention has the advantages of no pollution, convenience in operation, high selectivity of the product isophorone and the like, and belongs to the green and environment-friendly technology.
(2) In the scheme provided by the invention, the azeotropic bulkhead tower technology is adopted to directly separate water from the azeotrope such as water, isophorone, isopropylidene isomer and the like, thereby obviously reducing the separation difficulty of subsequent products, simplifying the process and saving the energy consumption.
(3) In the scheme provided by the invention, the mesitylene, the isophorone and the tetramer are separated and obtained by adopting a bulkhead tower technology, so that the purity of each product can be obviously improved while the separation process is simplified, the energy consumption is reduced, the cost is saved, and the like.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a flow chart of an apparatus for producing isophorone by vapor phase condensation of acetone in an embodiment of the present invention;
in the figure:
1: acetone raw material; 2: a vaporizer; 3: vaporized acetone raw material; 4: a heat exchanger; 5: acetone raw material after heat exchange; 6: a fixed bed reactor; 7: a reaction product; 8: a fixed bed reactor product after heat exchange with the raw material acetone; 9: an acetone recovery column; 10: acetone is recovered to obtain a gas-phase product at the top of the tower; 11: an acetone recovery tower condenser; 12: recycling the acetone; 13: an acetone recovery tower reboiler; 14: the mixture at the bottom of the acetone recovery tower; 15: a first divided wall column; 16: an azeotropic distillation zone; 17: a water purification zone; 18: a first divided wall column overhead vapor stream; 19: a first divided wall column condenser; 20: liquid separating tank; 21: supplementing an entrainer; 22: oil phase of the liquid separating tank; 23: separating the water phase in the liquid tank; 24: an intermediate reboiler; 25: waste water; 26: an azeotropic dividing wall column reboiler; 27: a first dividing wall column partition; 28: a bottoms stream of an azeotropic dividing wall column; 29: an mesityl oxide column; 30: the gas phase at the top of the mesityl oxide tower; 31: an mesityl oxide column condenser; 32: mesityl oxide; 33: an mesityl oxide column reboiler; 34: a bottom stream of an mesityl oxide column; 35: a second divided wall column; 36: a second divided wall column partition; 37: a second divided wall column common rectification section; 38: a common stripping section of a second divided wall column; 39: a first bulkhead column preliminary distillation zone; 40: a second bulkhead column sidetrack region; 41: a second bulkhead column overhead vapor product; 42: a second divided wall column condenser; 43: a mesitylene product; 44: an isophorone product; 45: a dividing wall column reboiler; 46: a tetramer.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
The invention provides equipment for preparing isophorone by acetone gas phase condensation, which comprises: an acetone recovery column 9, a first divided wall column (i.e., azeotropic divided wall column) 15, an mesityl oxide column 29, and a second divided wall column 35; wherein, the middle part of the acetone recovery tower is provided with a first feed inlet, and the bottom of the tower is provided with a first discharge outlet; a first bulkhead tower clapboard 27 is positioned on a central axis in the tower, an azeotropic distillation area 16 is positioned on the left side of the clapboard, a water purification area 17 is positioned on the right side of the clapboard, the middle part of the azeotropic distillation area is provided with a second feeding hole, the second feeding hole is connected with a first discharging hole through a pipeline, and the bottom of the first bulkhead tower is provided with a second discharging hole; in the mesityl oxide tower, a third feed inlet is arranged in the middle of the mesityl oxide tower, the third feed inlet is connected with the second discharge outlet through a pipeline, and a third discharge outlet is arranged at the bottom of the mesityl oxide tower; the second next door tower baffle 36 is located the center axis in the tower, second next door tower preliminary distillation district 39 is located the baffle left side, second next door tower sideline district 40 is located the baffle right side, second next door tower public distillation section 37 is located baffle upper portion, second next door tower public stripping section 38 is located the baffle lower part, the middle part in preliminary distillation district is provided with the fourth feed inlet, the fourth feed inlet passes through the pipe connection with the third discharge gate, the middle part in sideline district is provided with the fourth discharge gate. Wherein the theoretical plate number of the acetone recovery tower is 40-65, and the theoretical plate number of the mesityl oxide tower is 25-50; in the first dividing wall tower, the theoretical plate number of the water purification area is 10-20, the theoretical plate number of the azeotropic rectification area is 30-50, and the first dividing wall tower is an azeotropic dividing wall tower; in the second dividing wall tower, the number of theoretical plates in the initial distillation zone is 10-25, the number of theoretical plates in the side line zone is 15-30, the number of theoretical plates in the public rectification section is 5-15, and the number of theoretical plates in the public stripping section is 4-25.
Preferably, one or more of a vaporizer, a heat exchanger, a condenser, a reboiler and a liquid separation tank are further provided between the acetone recovery column, the first divided wall column, the mesityl oxide column and the second divided wall column.
Preferably, in the second partition wall tower, the extraction position of the fourth discharge port is 5 th to 15 th tower plates in the side line area.
Specifically, fig. 1 is a flow chart of an apparatus for preparing isophorone by vapor phase condensation of acetone in the embodiment of the present invention; as shown in fig. 1, the process flow of the present invention comprises:
the method comprises the following steps of heating an acetone raw material 1 by a vaporizer 2 to obtain a vaporized acetone raw material 3, exchanging heat between the vaporized acetone raw material and a reaction product 7 of a fixed bed reactor 6 by a heat exchanger 4, feeding the heat exchanged acetone raw material 5 into the fixed bed reactor, and then carrying out condensation reaction under the action of a catalyst to generate a product: isophorone, by-products of mesitylene, tetramer and impurity water.
The method comprises the steps of enabling a fixed bed reactor product 8 subjected to heat exchange with raw material acetone to enter an acetone recovery tower 9 for acetone recovery, enabling an acetone recovery tower top gas phase product 10 to be subjected to acetone recovery, enabling the acetone recovery tower top gas phase product to pass through an acetone recovery tower condenser 11 and then to be circulated back to a vaporizer 2 for recycling, namely circulating acetone 12, enabling an acetone recovery tower bottom mixture 14 to pass through an acetone recovery tower reboiler 13 and then enter a first partition tower (namely an azeotropic partition tower) 15 for separation, enabling a first partition tower top gas phase material flow 18 to pass through a first partition tower condenser 19 and then enter a liquid separation tank 20, wherein 22 is a liquid separation tank oil phase, and 23 is a liquid separation tank water phase.
The supplementary entrainer 21 enters from the tower top liquid separation tank 20 of the azeotropic bulkhead tower 15, after the waste water 25 is removed in the azeotropic bulkhead tower, the tower bottom material flow 28 of the azeotropic bulkhead tower enters the mesityl oxide tower 29 for separation after passing through the azeotropic tower reboiler 26, and then the tower top gas phase 30 of the mesityl oxide tower passes through the mesityl oxide tower condenser 31 to obtain the high-purity mesityl oxide 32. Wherein 24 is an intermediate reboiler.
The bottom material flow 34 of the mesityl oxide tower enters a second bulkhead tower 35 for three-component separation after passing through a reboiler 33 of the mesityl oxide tower, high-purity mesitylene 43 is obtained after a gas-phase product 41 at the top of the second bulkhead tower passes through a condenser 42 of the second bulkhead tower, high-purity isophorone 44 is obtained in a side line area 40 of the second bulkhead tower, and a tetramer 46 is obtained from the bottom product of the second bulkhead tower passing through the reboiler 45 of the second bulkhead tower. The mass purities of the product isophorone 44, the byproduct mesityl oxide 32, the mesitylene 43 and the tetramer 46 which are finally obtained are all more than or equal to 99.6 percent.
The following description is given with reference to specific examples:
example one
The acetone raw material 1 is heated by a vaporizer 2 and then exchanges heat with a product 7 of a fixed bed reactor 6, and a material flow 5 after heat exchange enters the fixed bed reactor to carry out condensation reaction under the action of a catalyst to generate a product isophorone, and byproducts of mesitylene, tetramer and impurity water.
The product of the reactor and the material flow 8 after heat exchange of the raw material acetone enter an acetone recovery tower 9 for acetone recovery, high-purity acetone 12 obtained at the top of the tower is recycled to the vaporizer 2 for reuse, and a mixture 14 at the bottom of the tower enters an azeotropic partition tower 15 for separation.
The complementary entrainer 21 enters into the liquid separation tank 20 at the top of the azeotropic bulkhead tower 15, after the water 25 is removed in the azeotropic bulkhead tower 15, the mixture 28 at the bottom of the tower enters into the mesityl oxide tower 29 for separation, the high-purity mesityl oxide 32 is obtained at the top of the tower, and the mixture at the bottom of the tower enters into the second bulkhead tower 35 for three-component separation.
High-purity mesitylene 43 is obtained at the top of the second dividing wall tower 35, high-purity isophorone 44 is obtained at the lateral line, and tetramer 46 is obtained at the bottom of the tower.
In the embodiment, the entrainer is ethyl acetate, the operating pressure of the fixed bed reactor 6 is 0.5atm, and the temperature is 250 ℃; the acetone recovery tower 9 is a plate tower, the theoretical plate number is 40, the operation pressure is 0.5atm, the tower top temperature is 39 ℃, and the tower bottom temperature is 75 ℃. The azeotropic dividing wall tower 15 is a packed tower, the theoretical plate number of the water purification area 17 is 10, the theoretical plate number of the azeotropic rectification area 16 is 30, the operation pressure is 0.5atm, the tower top temperature is 50 ℃, and the tower bottom temperature is 70 ℃. The mesityl oxide tower 29 is a plate tower, the theoretical plate number is 25, the operation pressure is 0.15atm, the tower top temperature is 40 ℃, and the tower bottom temperature is 120 ℃. The second divided wall column 35 is a plate column, the number of plates of the first distillation section 39 is 10, the number of theoretical plates of the side line zone 40 is 15, the number of theoretical plates of the common distillation section 37 is 5, the number of theoretical plates of the common stripping section 38 is 4, the operating pressure is 0.1atm, the temperature at the top of the column is 45 ℃, the temperature at the bottom of the column is 120 ℃, and the position where the side line isophorone stream 44 is extracted is the 5 th plate of the side line zone 40. The flow rates and compositions of mesitylene 43, isophorone 44, and tetramer 46, and mesitylene 32 are shown in Table 1.
Table 1 flow and composition of streams 32, 43, 44 and 46 in example one
As can be seen from Table 1, the mass purities of the target product isophorone and the byproducts mesitylene, mesitylene and tetramer were all 0.9960 or more.
Example two
The process flow in this embodiment is the same as that in the first embodiment, except that: the entrainer adopts n-butyl acetate, the operating pressure of the fixed bed reactor 6 is 1.0atm, and the temperature is 335 ℃; the acetone recovery tower 9 is a packed tower, the theoretical plate number is 50, the operation pressure is 1.0atm, the tower top temperature is 45 ℃, and the tower bottom temperature is 80 ℃. The azeotropic dividing wall column 15 is a plate column, the theoretical plate number of the water purification area 17 is 16, the theoretical plate number of the azeotropic rectification area 16 is 42, the operation pressure is 1.2atm, the temperature of the top of the column is 62 ℃, and the temperature of the bottom of the column is 83 ℃. The mesityl oxide tower 29 is a packed tower, the theoretical plate number is 35, the operation pressure is 0.25atm, the tower top temperature is 47 ℃, and the tower bottom temperature is 132 ℃. The second divided wall tower 35 is a packed tower, the number of the trays in the first stage 39 is 14, the number of the theoretical trays in the side line area 40 is 19, the number of the theoretical trays in the common rectification stage 37 is 8, the number of the theoretical trays in the common stripping stage 38 is 10, the operating pressure is 0.24atm, the temperature at the top of the tower is 56 ℃, the temperature at the bottom of the tower is 135 ℃, and the position where the side line isophorone stream 44 is extracted is the 8 th tray in the side line area 40. The flow rates and compositions of mesitylene 43, isophorone 44, and tetramer 46, and mesitylene 32 are shown in Table 2.
TABLE 2 flow rates and compositions of streams 32, 43, 44 and 46 in example two
As can be seen from Table 2, the target products isophorone and by-products mesitylene, tetramer all had mass purities of 0.9960 or more.
EXAMPLE III
The process flow in this embodiment is the same as that in the first embodiment, except that: the entrainer is isobutyl formate, the operating pressure of the fixed bed reactor 6 is 3.5atm, and the temperature is 360 ℃. The acetone recovery tower 9 is a plate tower, the theoretical plate number is 60, the operation pressure is 2atm, the tower top temperature is 55 ℃, and the tower bottom temperature is 95 ℃. The azeotropic dividing wall column 15 is a plate column, the theoretical plate number of the water purification area 17 is 17, the theoretical plate number of the azeotropic rectification area 16 is 45, the operation pressure is 2atm, the temperature of the top of the column is 70 ℃, and the temperature of the bottom of the column is 92 ℃. The mesityl oxide tower 29 is a packed tower, the theoretical plate number is 46, the operation pressure is 0.75atm, the tower top temperature is 60 ℃, and the tower bottom temperature is 159 ℃. The second divided wall column 35 is a plate column, the number of plates of the first distillation section 39 is 21, the number of theoretical plates of the side line zone 40 is 26, the number of theoretical plates of the common distillation section 37 is 12, the number of theoretical plates of the common stripping section 38 is 21, the operating pressure is 0.78atm, the top temperature of the column is 85 ℃, the bottom temperature of the column is 160 ℃, and the position where the side line isophorone stream 44 is extracted is the 13 th plate of the side line zone 40. The flow rates and compositions of mesitylene 43, isophorone 44, and tetramer 46, and mesitylene 32 are shown in Table 3.
TABLE 3 flow and composition of streams 32, 43, 44 and 46 in example III
As can be seen from Table 3, the mass purities of the target product isophorone and the by-products mesitylene, and tetramer were all 0.9960 or more.
Example four
The process flow in this embodiment is the same as that in the first embodiment, except that: the entrainer adopts n-propyl formate, the operating pressure of the fixed bed reactor 6 is 6atm, and the temperature is 450 ℃. The acetone recovery tower 9 is a packed tower, the theoretical plate number is 65, the operation pressure is 2.5atm, the tower top temperature is 66 ℃, and the tower bottom temperature is 105 ℃. The azeotropic dividing wall tower 15 is a packed tower, the theoretical plate number of the water purification area 17 is 20, the theoretical plate number of the azeotropic rectification area 16 is 50, the operation pressure is 2.5atm, the tower top temperature is 80 ℃, and the tower bottom temperature is 105 ℃. The mesityl oxide tower 29 is a packed tower, the theoretical plate number is 50, the operation pressure is 1.0atm, the tower top temperature is 69 ℃, and the tower bottom temperature is 165 ℃. The second divided wall column 35 is a plate column, the number of plates in the first stage 39 is 25, the number of theoretical plates in the side line zone 40 is 30, the number of theoretical plates in the common rectification stage 37 is 15, the number of theoretical plates in the common stripping stage 38 is 25, the operating pressure is 1.0atm, the temperature at the top of the column is 95 ℃, the temperature at the bottom of the column is 175 ℃, and the position where the side line isophorone stream 44 is extracted is the 15 th plate in the side line zone 40. The flow rates and compositions of mesitylene 43, isophorone 44, and tetramer 46, and mesitylene 32 are shown in Table 4.
TABLE 4 flow and composition of streams 32, 43, 44 and 46 in example four
As can be seen from Table 4, the mass purities of the target product isophorone and the by-products mesitylene, and tetramer were all 0.9960 or more.
Of course, other reaction conditions, numbers of plates, and the like are possible, in addition to the cases exemplified in examples one to four.
The invention adopts novel separation technologies such as a partition tower and the like, and can effectively separate and recover various products in the acetone condensation reaction: main products of isophorone, byproducts of mesitylene, tetramer and the like, and the mass purity of each product is more than or equal to 99.60 percent; in addition, the invention obviously simplifies the process flow of preparing isophorone by acetone condensation and reduces equipment investment and energy consumption.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., 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 are not necessarily intended to 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. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (4)
1. The method for preparing isophorone by acetone gas phase condensation is characterized by comprising the following steps of: the device comprises an acetone recovery tower, a first partition tower, an mesityl oxide tower and a second partition tower;
the middle part of the acetone recovery tower is provided with a first feeding hole, and the bottom of the acetone recovery tower is provided with a first discharging hole;
in the first bulkhead tower, a partition plate is positioned on a central axis in the tower, an azeotropic distillation area is positioned on the left side of the partition plate, a water purification area is positioned on the right side of the partition plate, a second feed inlet is arranged in the middle of the azeotropic distillation area, the second feed inlet is connected with the first discharge outlet through a pipeline, and a second discharge outlet is arranged at the bottom of the first bulkhead tower;
in the mesityl oxide tower, a third feed inlet is arranged in the middle of the mesityl oxide tower, the third feed inlet is connected with the second discharge outlet through a pipeline, and a third discharge outlet is arranged at the bottom of the mesityl oxide tower;
in the second bulkhead tower, the baffle is located the center axis in the tower, and the preliminary distillation district is located the baffle left side, and the lateral line position is on the baffle right side, and public rectification section is located baffle upper portion, and public stripping section is located the baffle lower part, the middle part in preliminary distillation district is provided with the fourth feed inlet, the fourth feed inlet with the third discharge gate passes through pipe connection, the middle part in lateral line district is provided with fourth discharge gate
The method is completed by adopting the equipment, and specifically comprises the following steps:
s101: feeding the product of the acetone condensation reaction into an acetone recovery tower through a first feeding hole to recover acetone, and then obtaining a first mixture at a first discharging hole;
s102: the first mixture enters a first bulkhead tower through a second feed inlet for dehydration treatment, and then a second mixture is obtained at a second discharge outlet;
s103: feeding the second mixture into an mesityl oxide tower, and then obtaining a third mixture at a third discharge hole;
s104: and feeding the third mixture into a second partition tower, and then obtaining isophorone at the fourth discharge hole.
2. The process for producing isophorone according to claim 1, wherein:
before S101, the method further includes step S100: reacting raw material acetone in a fixed bed reactor under the action of a catalyst, and then exchanging heat between a product of the fixed bed reactor and the raw material acetone to obtain a product of the acetone condensation reaction.
3. The process for producing isophorone according to claim 1, which further comprises supplementing an azeotropic agent in the first divided wall column;
the entrainer comprises one or more of n-propyl formate, n-butyl acetate, ethyl acetate and isobutyl formate.
4. The method for preparing isophorone by acetone vapor phase condensation according to any one of claims 1-3, wherein:
in the S101, the temperature of the top of the acetone recovery tower is 39-66 ℃, the temperature of the bottom of the acetone recovery tower is 75-105 ℃, and the operating pressure is 0.5-2.5 atm;
in the S102, the operating pressure of the first bulkhead tower is 0.5-2.5 atm, the tower top temperature is 50-80 ℃, and the tower bottom temperature is 70-105 ℃;
in the S103, the temperature of the top of the mesityl oxide tower is 40-69 ℃, the temperature of the bottom of the mesityl oxide tower is 120-165 ℃, and the operating pressure is 0.15-1.0 atm;
in the S104, the operating pressure of the second partition tower is 0.1-1.0 atm, the tower top temperature is 45-95 ℃, and the tower bottom temperature is 120-175 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710766032.6A CN107573227B (en) | 2017-08-30 | 2017-08-30 | Equipment and method for preparing isophorone by acetone gas phase condensation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710766032.6A CN107573227B (en) | 2017-08-30 | 2017-08-30 | Equipment and method for preparing isophorone by acetone gas phase condensation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107573227A CN107573227A (en) | 2018-01-12 |
| CN107573227B true CN107573227B (en) | 2020-07-21 |
Family
ID=61030167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710766032.6A Active CN107573227B (en) | 2017-08-30 | 2017-08-30 | Equipment and method for preparing isophorone by acetone gas phase condensation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107573227B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108947777B (en) * | 2018-05-31 | 2021-09-10 | 江苏焕鑫新材料股份有限公司 | Enrichment and separation process of low-concentration multi-component phenol-containing mixture |
| CN108911956B (en) * | 2018-06-20 | 2021-10-08 | 江苏焕鑫新材料股份有限公司 | Purification process of cracking by-product in condensation reaction |
| CN111377806B (en) * | 2018-12-27 | 2022-07-12 | 万华化学集团股份有限公司 | Post-treatment process for preparing isophorone by acetone liquid phase condensation method |
| CN111377807B (en) * | 2018-12-27 | 2023-03-03 | 万华化学集团股份有限公司 | Preparation method of isophorone with low color number and low acid value |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633610A (en) * | 2009-08-13 | 2010-01-27 | 浙江大学 | Method for preparing alpha-isophorone |
| CN102159291A (en) * | 2008-09-17 | 2011-08-17 | 巴斯夫欧洲公司 | Devices and method for continuous distillative separation of mixture containing one or more alkanolamine(s) |
| CN106748792A (en) * | 2016-11-15 | 2017-05-31 | 中国石油大学(华东) | The method and apparatus that azeotropic reaction rectification method produces methyl ethyl carbonate |
-
2017
- 2017-08-30 CN CN201710766032.6A patent/CN107573227B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102159291A (en) * | 2008-09-17 | 2011-08-17 | 巴斯夫欧洲公司 | Devices and method for continuous distillative separation of mixture containing one or more alkanolamine(s) |
| CN101633610A (en) * | 2009-08-13 | 2010-01-27 | 浙江大学 | Method for preparing alpha-isophorone |
| CN106748792A (en) * | 2016-11-15 | 2017-05-31 | 中国石油大学(华东) | The method and apparatus that azeotropic reaction rectification method produces methyl ethyl carbonate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107573227A (en) | 2018-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107573227B (en) | Equipment and method for preparing isophorone by acetone gas phase condensation | |
| CN101265158B (en) | Method for producing 1,6-hexandiol | |
| CN101998945B (en) | Process and apparatus for efficient recovery of dichlorohydrins | |
| CN108033875B (en) | System and method for continuously producing glycol ether | |
| US8664453B2 (en) | Multi-stage process and apparatus for recovering dichlorohydrins | |
| CN104761429B (en) | A kind of method for producing dimethyl carbonate and ethylene glycol | |
| CN101328119A (en) | Synthetic process method of methyl acetate and apparatus thereof | |
| CN105037094B (en) | A kind of energy coupling rectificating method of acetate preparation of ethanol by hydrogenating | |
| CN107628946A (en) | The method and device of reactive distillation film device coupling production ethyl acetate in high purity | |
| CN101367732A (en) | Process and apparatus for preparing diethyl carbonate | |
| CN107108413A (en) | Prepare device of glycol and preparation method thereof | |
| WO2020029753A1 (en) | Production process of 2,2-dimethyl-1,3-propanediol | |
| CN104529763A (en) | Process and device for synthesizing ethyl formate with reactive distillation dividing wall column | |
| CN109180435A (en) | A kind of device and method preparing isopropanol from recuperation of heat reactive distillation | |
| CN101657404B (en) | Process and apparatus for recovery of dichlorohydrins via codistillation | |
| CN103467263A (en) | Preparation method of isophorone | |
| WO2020015321A1 (en) | Method and device for separating isopropanol | |
| CN101998944B (en) | Multi-stage process and apparatus for recovering dichlorohydrins | |
| CN115160109B (en) | Method for separating glycol and glycol diacetate by using sulfolane as entrainer | |
| JP6027723B2 (en) | Method for producing C1-C4 alkyl nitrite | |
| CN109956849B (en) | Method for preparing ethylene glycol diacetate and sec-butyl alcohol, catalytic system and device | |
| KR100339973B1 (en) | Method and apparatus of methyl acetate hydrolysis | |
| CN115282913A (en) | Reaction system and method for preparing methyl propionate | |
| CN109646977B (en) | Reactive distillation coupling tower and application thereof in preparation of formic acid | |
| CN108299155B (en) | Method for producing cyclopentanol and cyclopentanone from cyclopentene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |