CN212347756U - Methyl phenyl carbonate reaction rectifying tower device - Google Patents
Methyl phenyl carbonate reaction rectifying tower device Download PDFInfo
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- CN212347756U CN212347756U CN202020595215.3U CN202020595215U CN212347756U CN 212347756 U CN212347756 U CN 212347756U CN 202020595215 U CN202020595215 U CN 202020595215U CN 212347756 U CN212347756 U CN 212347756U
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Abstract
The utility model discloses a methyl phenyl carbonate reaction rectifying tower device, which comprises a reaction rectifying tower (1), a condenser (2) and a reboiler (3), wherein a tower tray (11) of the reaction rectifying tower (1) comprises a baffle plate (111), an injection cover (112) and a separation plate (113), wherein the baffle plate (111) is provided with a circulation hole (1111) for dimethyl carbonate to pass through; the bottom of the spraying cover (112) is provided with an opening, the spraying cover is arranged above the baffle (111) and covers the circulating hole (1111), and the caliber of the spraying cover is at least partially reduced gradually from bottom to top; the separation plate (113) covers the upper part of the spray cover (112); the wall surfaces of the spray cover (112) and the separating plate (113) are provided with sieve holes. Compared with the prior art, the utility model discloses a methyl phenyl carbonate reaction rectifying column device can improve methyl phenyl carbonate's selectivity.
Description
Technical Field
The utility model relates to a methyl phenyl carbonate production technical field specifically indicates a methyl phenyl carbonate reaction rectifying column device.
Background
In recent years, polycarbonate is widely used in the fields of electronic and electric appliances, machinery, aviation, transportation, construction, agriculture, textile, medical treatment, and the like, and is in short supply, and polycarbonate is a product obtained by transesterification between bisphenol a and diphenyl carbonate, and therefore, demand for diphenyl carbonate as a raw material thereof has increased, and research on a method for synthesizing diphenyl carbonate has been a focus of attention. The diphenyl carbonate is also generated by ester exchange reaction, the methyl phenyl carbonate is an intermediate product of phenol and dimethyl carbonate which are synthesized into the diphenyl carbonate by ester exchange method, the specific flow is that the phenol and the dimethyl carbonate are generated into the methyl phenyl carbonate by ester exchange method, the methyl phenyl carbonate can generate ester exchange reaction to generate the dimethyl carbonate and the diphenyl carbonate, therefore, the selectivity of the methyl phenyl carbonate has great relation to the synthesis of the diphenyl carbonate. Wherein, the selectivity is also called as the specificity of the reaction. If a chemical reaction can produce multiple products simultaneously, where one product is most desirable, the magnitude of the yield of that product represents the selectivity of the reaction. Product selectivity is the amount of target product produced/reactant consumption.
The method for preparing the methyl phenyl carbonate at present mainly comprises three methods, wherein phenyl chloroformate is reacted with methanol to generate the methyl phenyl carbonate, and the method has the defects that the highly toxic phenyl chloroformate is used, and the methyl phenyl carbonate can be obtained by a product after the reaction through multiple operations, so the method is rarely adopted in the prior art. Secondly, methyl phenyl carbonate is generated by taking dimethyl carbonate and diphenyl carbonate as raw materials (see patent with publication numbers of CN102531908A and CN103467283A), the operation procedures of the process are complex, multiple condensation is needed, and the methyl phenyl carbonate can be obtained through reaction. Thirdly, methyl phenyl carbonate is produced by ester exchange method (see patent with publication number CN104478711A), and methyl phenyl carbonate is directly obtained by the reaction of phenol and dimethyl carbonate.
The transesterification method is considered to be the most suitable method for synthesizing methyl phenyl carbonate in the present polycarbonate device, and the transesterification reaction refers to the reaction of an ester and an alcohol/acid/ester under the catalysis of the reaction to generate a new ester and a new alcohol/acid/ester. The reaction equation for the transesterification of dimethyl carbonate and phenol is:
the resulting methyl phenyl carbonate itself also undergoes transesterification (disproportionation):
in the products generated by the ester exchange process, the selectivity of the methyl phenyl carbonate is about 90 percent, and further space is provided for improvement. The following techniques, although greatly improved on the synthesis of methyl phenyl carbonate, still have drawbacks.
For example, in patent "preparation method of methyl phenyl carbonate" with publication number CN201110449387.5 (publication number CN102531908A), the raw materials of the method are dimethyl carbonate and diphenyl carbonate, and the reaction is catalyzed by a catalyst to produce methyl phenyl carbonate, the purity is increased to 99.1%, the patent does not mention the final selectivity of the product, and it can not achieve very high requirement in product selectivity, and it belongs to batch reaction, and is not suitable for industrial production and large-scale synthesis.
For example, in patent "preparation method of methyl phenyl carbonate" with patent application No. CN201110449387.5 (publication No. CN103467283A), methyl phenyl carbonate is finally obtained by separation and purification using dimethyl carbonate and diphenyl carbonate as raw materials through double-column coupling. Although the method is a continuous reaction, the purity is as high as 99.9 percent, the patent does not mention the final selectivity of the product, the product selectivity does not meet high requirements, and a plurality of condensers, buffer tanks and other equipment are added through double-tower coupling, so the operation is complex and the energy consumption is high.
For example, in patent "preparation method of methyl phenyl carbonate" with patent application No. CN201410726718.9 (publication No. CN104478711A), phenol and dimethyl carbonate are used as raw materials, and an experiment is carried out in a microreactor, so that the selectivity of the final methyl phenyl carbonate is 99.9%. This method is data obtained in the laboratory and has not been practically industrially applied.
In the traditional process, a tray of a rectifying tower usually adopts a float valve tray, however, bubbles formed by the tray are large, the vapor-liquid contact surface is small, the mass transfer efficiency is low, more trays are usually needed to complete the separation requirement, in addition, because the bubbles are large, higher tray spacing is also needed to prevent entrainment, and generally, the height of the float valve tower is about 50 meters, so that the selectivity of methyl phenyl carbonate cannot be ensured.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that to prior art's current situation, provide a methyl phenyl carbonate reaction rectifying column device that can improve methyl phenyl carbonate's selectivity.
The utility model provides a technical scheme that above-mentioned technical problem adopted does: a methyl phenyl carbonate reaction rectifying column device is characterized in that: comprises that
The reaction rectifying tower is internally provided with a plurality of tower trays at intervals along the height direction, the middle part of the reaction rectifying tower is provided with a first material inlet for phenol and catalyst to enter, the lower part of the reaction rectifying tower is provided with a second material inlet for dimethyl carbonate to enter, the side wall of the reaction rectifying tower is provided with a first material outlet for anisole to discharge, the top of the reaction rectifying tower is provided with a second material outlet for methanol, phenol and dimethyl carbonate to discharge, and the bottom of the reaction rectifying tower is provided with a third material outlet for methyl phenyl carbonate to discharge;
the condenser is arranged close to the top of the reactive distillation tower and is used for condensing the material distilled from the top of the reactive distillation tower; and
the reboiler is arranged close to the top of the reactive distillation tower and is used for vaporizing materials distilled from the bottom of the reactive distillation tower; the tray comprises
The baffle is provided with a circulation hole for the dimethyl carbonate to pass through;
the bottom of the spraying cover is provided with an opening, the spraying cover is arranged above the baffle plate and covers the circulation hole, and the caliber of the spraying cover is at least partially reduced gradually from bottom to top; and
a separation plate covering above the spray hood;
the wall surfaces of the spraying cover and the separating plate are provided with sieve holes.
In order to further improve the mass transfer efficiency, the condenser is arranged inside the reaction rectifying tower. In the traditional process, a tower top condenser of a rectifying tower is generally externally arranged on the tower top edge of the rectifying tower, the arrangement mode is not suitable for the system, and because the methyl phenyl carbonate in the system has high boiling point and high density, the methyl phenyl carbonate is easy to condense to form a dead zone, so that mass transfer is influenced.
The reboiler is arranged at two positions:
the first scheme employs a conventional extra-column reboiler: the reboiler is arranged outside the reactive distillation column, the bottom of the reboiler is provided with a third material inlet for dimethyl carbonate liquid phase to enter and a fourth material inlet for methyl phenyl carbonate to enter, the fourth material inlet is communicated with the third material outlet, the top of the reboiler is provided with a fourth material outlet for gas phase to discharge, and the fourth material outlet is communicated with the second material inlet.
The second solution employs a built-in reboiler: the reboiler is arranged in the reaction rectifying tower. Through built-in with the reboiler, saved casing and connecting line, its simple structure, the cost is lower than the outer reboiler of traditional tower, and direct heating has avoided the dwell time of material in the reboiler casing simultaneously in the tower, thereby causes local material not to circulate and takes place the reunion phenomenon.
In order to ensure that the reaction temperature is reached when the materials are fed, the method also comprises
The tube side inlet of the first heat exchanger is used for allowing phenol and a catalyst to enter, and the tube side outlet is communicated with the first material inlet; and
and a tube pass inlet of the second heat exchanger is used for allowing dimethyl carbonate to enter, and a tube pass outlet is communicated with the third material inlet or the second material inlet.
In order to recover the heat of the condenser for the heat exchanger and reduce the energy consumption, the heat exchanger also comprises a circulating pump for conveying a heat exchange medium;
the shell pass outlet of the condenser is respectively communicated with the shell pass inlets of the first heat exchanger and the second heat exchanger;
the shell side outlets of the first heat exchanger and the second heat exchanger are both communicated with the inlet of the circulating pump;
and the outlet of the circulating pump is communicated with the shell side inlet of the condenser.
In the traditional process, the feeding of a rectifying tower usually directly enters the rectifying tower, the heat of a reboiler at the bottom of the tower is used for heating materials to reach the reaction temperature, or a heat exchanger is arranged before the feeding, the materials are preheated by public engineering steam, usually, extra energy consumption is caused by the preheating mode, the heat recovered by a condenser at the top of the tower in the application can be used for preheating the feeding, the energy consumption is reduced, the temperature and the viscosity of the materials of the system are in a nonlinear relation, the viscosity can be greatly improved by increasing the temperature, the reaction and the separation are simultaneously carried out in the rectifying tower, the boiling point of the methyl phenyl carbonate generated by the reaction is high, the density is low, the reactants are required to be diffused as soon as possible, the agglomeration phenomenon is caused as few as possible, the specific surface area of the reaction and the vapor-liquid contact is as large as possible, the reaction and the vapor-. If the cold material enters the rectifying tower, the temperature of the material at the inlet side is instantly reduced after the material is contacted, partial material agglomeration is formed, the agglomerate reacts with the surroundings, the mass transfer is slow, the temperature in the agglomerate is slowly transferred, almost no reaction is caused, the reaction selectivity is influenced if the temperature is light, and the blockage problem is caused if the temperature is heavy. The problem is improved only by increasing the feeding temperature, and engineering verification proves that the influence can be eliminated only by reaching 150 ℃, the temperature of the tower top steam of the rectifying tower can be just matched with the temperature interval, but the tower top steam contains methyl phenyl carbonate steam and is directly heated to cause series problems such as blockage, other media are adopted as a refrigerant and a heating medium in the rectifying tower, and the polymer blockage and agglomeration problems are effectively avoided.
In order to ensure the heat exchange effect of the condenser, the condenser also comprises
The outlet of the heat exchange medium feeding device is communicated with the shell pass inlet of the condenser and is used for feeding a supplemented part of heat exchange medium into the shell pass of the condenser;
and an inlet of the heat exchange medium discharging device is communicated with the shell pass outlet of the condenser and is used for receiving part of the heat exchange medium in the shell pass of the condenser.
Through the device, the feeding and discharging of the heat exchange medium in the shell pass of the condenser are increased, and the device is used for preventing special conditions such as poor heat exchange effect.
Preferably, the first heat exchanger and the second heat exchanger are at least one of a shell-and-tube heat exchanger, a plate heat exchanger and a spiral-tube plate heat exchanger.
In order to avoid entrainment and influence on mass transfer, a certain separation height is required, the condenser is arranged above the tray positioned at the topmost part in the trays, and the distance between the condenser and the tray is 1-2 times of the distance between adjacent trays, so that the purity of a product at the top of the tower and the selectivity of methyl phenyl carbonate at the bottom of the tower can be improved.
Compared with the prior art, the utility model has the advantages of: by optimizing the structure of the tray, liquid in the tower is sprayed to the baffle in a spraying mode, the liquid is pulled into a liquid film, and the liquid film is crushed and rises to the separation plate for gas-liquid separation, so that the mass transfer efficiency can be improved, and the selectivity of the methyl phenyl carbonate can be improved. In addition, the waste heat recovery aspect is also greatly improved, the energy consumption is saved, and the product quality is improved.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment 1 of a methyl phenyl carbonate reaction rectifying tower device of the present invention;
FIG. 2 is a schematic structural diagram of a tray in example 1 of a methyl phenyl carbonate reaction rectifying column device according to the present invention;
FIG. 3 is a schematic structural diagram of an embodiment 2 of the apparatus of the present invention for rectifying a methyl phenyl carbonate reaction;
FIG. 4 is a schematic structural diagram of example 3 of the apparatus for rectifying a methyl phenyl carbonate reaction according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
Example 1:
as shown in FIGS. 1 and 2, the present invention is a first preferred embodiment of the apparatus of the present invention for rectifying reaction of methyl phenyl carbonate. The methyl phenyl carbonate reaction rectifying tower device comprises a reaction rectifying tower 1, a condenser 2, a reboiler 3, a first heat exchanger 4, a second heat exchanger 5 and a circulating pump 6.
The reaction rectifying tower comprises a reaction rectifying tower 1, a plurality of trays 11 arranged inside the reaction rectifying tower 1 at intervals along the height direction, a first material inlet 12 arranged in the middle of the reaction rectifying tower 1, a second material inlet 13 arranged at the lower part of the reaction rectifying tower 1, a first material outlet 14 for discharging anisole arranged on the side wall of the reaction rectifying tower 1, a second material outlet 15 for discharging methanol, phenol and dimethyl carbonate arranged at the top of the reaction rectifying tower 1, and a third material outlet 16 for discharging methyl phenyl carbonate arranged at the bottom of the reaction rectifying tower 1. In this embodiment, the tray 11 includes a baffle 111, an injection hood 112, and a separation plate 113, and the baffle 111 is provided with a circulation hole 1111 for passing dimethyl carbonate; the bottom of the injection cover 112 is provided with an opening and is arranged above the baffle plate 111, the injection cover 112 covers the circulation hole 1111, and the caliber of the injection cover 112 at least partially reduces gradually from bottom to top; a separation plate 113 is covered above the ejection hood 112; the spray cover 112 and the separating plate 113 have sieve holes on their wall surfaces. As shown in FIG. 4, dimethyl carbonate is brought into counter-current contact with phenol from the bottom up and reacted in the tray 11.
The condenser 2 is arranged close to the top of the reactive distillation column 1, arranged inside the reactive distillation column 1 and used for condensing the material distilled from the top of the reactive distillation column 1. In this embodiment, the condenser 2 is installed above the tray 11 positioned at the topmost part among the trays 11, and the interval between the condenser 2 and the tray 11 is 1 to 2 times the interval between the adjacent trays 11.
The reboiler 3 is arranged near the bottom of the reactive distillation column 1, is arranged outside the reactive distillation column 1, and is used for vaporizing the material distilled from the bottom of the reactive distillation column 1. The bottom of the reboiler 3 is provided with a third material inlet 31 for dimethyl carbonate liquid phase and a fourth material inlet 32 for methyl phenyl carbonate, the fourth material inlet 32 is communicated with the third material outlet 16, the top of the reboiler 3 is provided with a fourth material outlet 33 for gas phase discharge, and the fourth material outlet 33 is communicated with the second material inlet 13.
The tube side inlet of the first heat exchanger 4 is used for allowing phenol and a catalyst to enter, the tube side outlet of the first heat exchanger 4 is communicated with the first material inlet 12, the shell side inlet of the first heat exchanger 4 is communicated with the shell side outlet of the condenser 2, and the shell side outlet of the first heat exchanger 4 is communicated with the inlet of the circulating pump 6.
The tube-side inlet of the second heat exchanger 5 is used for feeding dimethyl carbonate, the tube-side outlet of the second heat exchanger 5 is communicated with the third material inlet 31, the shell-side inlet of the second heat exchanger 5 is communicated with the shell-side outlet of the condenser 2, and the shell-side outlet of the second heat exchanger 5 is communicated with the inlet of the circulating pump 6.
And the circulating pump 6 is used for conveying a heat exchange medium, and an outlet of the circulating pump 6 is communicated with a shell pass inlet of the condenser 2.
The working principle of the embodiment is as follows: after being mixed, phenol and a catalyst enter a first heat exchanger 4 for preheating, then enter a first material inlet 12 of a reaction rectifying tower 1, dimethyl carbonate enters a second heat exchanger 5 for preheating, then enter a reboiler 3, then enter a second material inlet of the reaction rectifying tower 1, the two materials react inside the reaction rectifying tower 1, generated products are separated, ascending steam in the reaction rectifying tower 1 directly enters a tube pass of a condenser 2 to exchange heat with a heat exchange medium in a shell pass for condensation, the heated heat exchange medium enters shell passes (flows in from the top and flows out from the bottom) of the first heat exchanger 4 and the second heat exchanger 5 to preheat the materials in the tube pass (flows in from the bottom and flows out from the bottom), and the cooled heat exchange medium enters the shell pass of the condenser 2 again through a circulating pump 6 to form closed cycle.
Example 2:
as shown in FIG. 3, it is a second preferred embodiment of the apparatus of the present invention for rectifying reaction of methyl phenyl carbonate. The difference from example 1 is that:
in this embodiment, the methyl phenyl carbonate reaction rectifying tower device further includes a heat exchange medium feeding device 7 and a heat exchange medium discharging device 8. An outlet of the heat exchange medium feeding device 7 is communicated with a shell pass inlet of the condenser 2 and is used for feeding a supplement part of heat exchange medium into a shell pass of the condenser 2; an inlet of the heat exchange medium discharging device 8 is communicated with a shell pass outlet of the condenser 2 and is used for receiving part of the heat exchange medium in the shell pass of the condenser 2. Through the device, the feeding and discharging of the heat exchange medium in the shell pass of the condenser 2 are increased, and the special conditions such as poor heat exchange effect are prevented from being adopted.
Example 3:
as shown in FIG. 4, it is a third preferred embodiment of the methyl phenyl carbonate reaction rectifying tower device of the present invention. The difference from example 1 is that:
in this embodiment, the reboiler 3 is disposed inside the reactive distillation column 1, and the tube-side outlet of the second heat exchanger 5 is directly communicated with the second material inlet 13.
Comparative example 1:
the difference from example 1 is that: tray 11 is a conventional float valve tray.
Comparative example 2:
the difference from example 1 is that: the condenser 2 is provided outside the reactive distillation column 1.
Comparative example 3:
the difference from example 1 is that: the first heat exchanger 4 and the second heat exchanger 5 are not provided.
The results of the performance tests of all examples and comparative examples are shown in table 1.
TABLE 1
The test method comprises the following steps: mixing dimethyl carbonate and phenol according to a molar ratio of 2:1, feeding the mixture into a reaction rectifying tower 1, and generating a mixture of dimethyl carbonate, phenol, anisole, methanol and methyl phenyl carbonate under the action of a catalyst, wherein the reaction temperature of the rectifying tower is 270 ℃, the pressure is 550kPaG, and the feeding amount of dimethyl carbonate is 90m3H phenol feed 47m3The reaction mixture is primarily separated in a reaction rectifying tower 1, methanol, phenol and dimethyl carbonate are distilled from the top of a rear tower, anisole is taken out from the side line, and methyl phenyl carbonate is taken out from the bottom of the tower.
As can be seen from Table 1, the methyl phenyl carbonate reaction rectification system can remarkably improve the selectivity of methyl phenyl carbonate, greatly improve the aspect of waste heat recovery, save energy consumption and improve the product quality.
Claims (10)
1. A methyl phenyl carbonate reaction rectifying column device is characterized in that: comprises that
The reaction rectifying tower (1) is internally provided with a plurality of trays (11) at intervals along the height direction, the middle part of the reaction rectifying tower is provided with a first material inlet (12) for phenol and catalyst to enter, the lower part of the reaction rectifying tower is provided with a second material inlet (13) for dimethyl carbonate to enter, the side wall of the reaction rectifying tower is provided with a first material outlet (14) for anisole to discharge, the top of the reaction rectifying tower is provided with a second material outlet (15) for methanol, phenol and dimethyl carbonate to discharge, and the bottom of the reaction rectifying tower is provided with a third material outlet (16) for methyl phenyl carbonate to discharge;
the condenser (2) is arranged close to the top of the reactive distillation tower (1) and is used for condensing the material distilled from the top of the reactive distillation tower (1); and
the reboiler (3) is arranged close to the top of the reactive distillation tower (1) and is used for vaporizing the material distilled from the bottom of the reactive distillation tower (1);
the tray (11) comprises
A baffle (111) provided with a circulation hole (1111) for the dimethyl carbonate to pass through;
the bottom of the spraying cover (112) is provided with an opening, the spraying cover is arranged above the baffle (111) and covers the circulating hole (1111), and the caliber of the spraying cover is at least partially reduced gradually from bottom to top; and
a separation plate (113) covering the upper side of the injection cover (112);
the wall surfaces of the spraying cover (112) and the separating plate (113) are provided with sieve holes.
2. The methyl phenyl carbonate reaction rectification column device according to claim 1, characterized in that: the condenser (2) is arranged in the reaction rectifying tower (1).
3. The methyl phenyl carbonate reaction rectification column device according to claim 2, characterized in that: the reboiler (3) is arranged outside the reactive distillation column (1), the bottom of the reboiler (3) is provided with a third material inlet (31) for dimethyl carbonate liquid phase to enter and a fourth material inlet (32) for methyl phenyl carbonate to enter, the fourth material inlet (32) is communicated with the third material outlet (16), the top of the reboiler (3) is provided with a fourth material outlet (33) for gas phase to be discharged, and the fourth material outlet (33) is communicated with the second material inlet (13).
4. The methyl phenyl carbonate reaction rectification column device according to claim 3, characterized in that: also comprises
The first heat exchanger (4), the tube side inlet is used for the phenol and catalyst to enter, the tube side outlet communicates with the first material inlet (12); and
and a tube pass inlet of the second heat exchanger (5) is used for allowing dimethyl carbonate to enter, and a tube pass outlet is communicated with the third material inlet (31).
5. The methyl phenyl carbonate reaction rectification column device according to claim 2, characterized in that: the reboiler (3) is arranged in the reaction rectifying tower (1).
6. The methyl phenyl carbonate reaction rectification column device according to claim 5, characterized in that: also comprises
The first heat exchanger (4), the tube side inlet is used for the phenol and catalyst to enter, the tube side outlet communicates with the first material inlet (12); and
and the tube side inlet of the second heat exchanger (5) is used for allowing dimethyl carbonate to enter, and the tube side outlet is communicated with the second material inlet (13).
7. The methyl phenyl carbonate reaction rectification column device according to claim 4 or 6, characterized in that: the heat exchanger also comprises a circulating pump (6) used for conveying a heat exchange medium;
the shell-side outlet of the condenser (2) is respectively communicated with the shell-side inlets of the first heat exchanger (4) and the second heat exchanger (5);
the shell-side outlets of the first heat exchanger (4) and the second heat exchanger (5) are communicated with the inlet of the circulating pump (6);
and the outlet of the circulating pump (6) is communicated with the shell side inlet of the condenser (2).
8. The methyl phenyl carbonate reaction rectification column device according to claim 7, characterized in that: also comprises
The outlet of the heat exchange medium feeding device (7) is communicated with the shell pass inlet of the condenser (2) and is used for feeding a supplement part of heat exchange medium into the shell pass of the condenser (2);
and an inlet of the heat exchange medium discharging device (8) is communicated with a shell pass outlet of the condenser (2) and is used for receiving part of the heat exchange medium in the shell pass of the condenser (2).
9. The methyl phenyl carbonate reaction rectification column device according to claim 4 or 6, characterized in that: the first heat exchanger (4) and the second heat exchanger (5) are at least one of a shell-and-tube heat exchanger, a plate heat exchanger and a spiral tube plate heat exchanger.
10. The methyl phenyl carbonate reaction rectification column device according to claim 1, characterized in that: the condenser (2) is arranged above the tray (11) which is positioned at the topmost part in the tray (11), and the distance between the condenser (2) and the tray (11) is 1-2 times of the distance between the adjacent trays (11).
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