CN220878863U - Preparation system of phenol acetone - Google Patents
Preparation system of phenol acetone Download PDFInfo
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- CN220878863U CN220878863U CN202322486056.XU CN202322486056U CN220878863U CN 220878863 U CN220878863 U CN 220878863U CN 202322486056 U CN202322486056 U CN 202322486056U CN 220878863 U CN220878863 U CN 220878863U
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- XDTRNDKYILNOAP-UHFFFAOYSA-N phenol;propan-2-one Chemical compound CC(C)=O.OC1=CC=CC=C1 XDTRNDKYILNOAP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000005728 strengthening Methods 0.000 claims abstract description 150
- 238000006243 chemical reaction Methods 0.000 claims abstract description 130
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 77
- 230000003647 oxidation Effects 0.000 claims abstract description 72
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 238000009833 condensation Methods 0.000 claims abstract description 6
- 230000005494 condensation Effects 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims description 49
- 229910052760 oxygen Inorganic materials 0.000 claims description 49
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 claims description 48
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 47
- 239000007789 gas Substances 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 19
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims 3
- 239000002994 raw material Substances 0.000 abstract description 16
- 230000035484 reaction time Effects 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 239000000498 cooling water Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000012045 crude solution Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Abstract
The utility model provides a preparation system of phenol acetone, which comprises an oxidation unit, wherein the oxidation unit comprises an oxidation tower, a first built-in strengthening unit is arranged in the oxidation tower, and the first built-in strengthening unit is arranged at the top end of the oxidation tower; the first built-in strengthening unit comprises a first strengthening reactor and a second strengthening reactor, the first strengthening reactor is arranged above the second strengthening reactor, a connecting pipe is arranged between the first strengthening reactor and the second strengthening reactor, and the first strengthening reactor is arranged above the liquid level; the condensation unit comprises a reaction kettle, a second built-in strengthening unit is arranged in the reaction kettle, and the second built-in strengthening unit is arranged at the top end of the reaction kettle. The phenol acetone preparation system can effectively improve the utilization rate of reaction raw materials, reduce the reaction time and the reaction temperature, and further effectively save energy consumption.
Description
Technical Field
The utility model belongs to the technical field of phenol acetone preparation, and particularly relates to a phenol acetone preparation system.
Background
Phenol is an organic chemical raw material with wide application, and the main preparation method is a cumene method. Wherein, cumene reacts with oxygen to generate cumene hydroperoxide (CHP for short), which is a key step for producing phenol acetone, and the specific reaction is as follows:
the main reaction:
Side reaction:
The existing industrial process for preparing phenol and acetone by oxidizing cumene mainly comprises the following steps: oxidizing cumene to generate CHP; concentrating CHP, and then carrying out acid decomposition to obtain crude phenol and acetone solution; and neutralizing the acid with the crude phenol and acetone solution, and rectifying and separating to obtain a phenol-acetone product.
However, the prior art reaction system for preparing phenol acetone involves the following problems:
the reactors of the first oxidation section and the oxidation section adopt bubbling reactors, the volume of bubbles in the reactors is overlarge, the bubbles cannot fully contact with liquid-phase cumene, and the reaction efficiency of the system is reduced;
Second, during the oxidation process, as the concentration of Cumene Hydroperoxide (CHP) increases, the reaction temperature increases while the CHP residence time increases and the side reaction products increase significantly.
In view of this, the present utility model has been made.
Disclosure of utility model
The utility model aims to provide a preparation system of phenol acetone, which combines an enhanced reaction technology into a phenol acetone preparation process, effectively improves the reaction efficiency of raw materials and the utilization rate of oxygen, and reduces the reaction temperature and the reaction time.
In order to achieve the above object of the present utility model, the following technical solutions are specifically adopted:
The utility model provides a preparation system of phenol acetone, which comprises:
the oxidation unit comprises an oxidation tower, a first built-in strengthening unit is arranged in the oxidation tower, and the first built-in strengthening unit is arranged at the top end of the oxidation tower;
The first built-in strengthening unit comprises a first strengthening reactor and a second strengthening reactor, the first strengthening reactor is arranged above the second strengthening reactor, a connecting pipe is arranged between the first strengthening reactor and the second strengthening reactor, and the first strengthening reactor is arranged above the liquid level;
A pre-reaction pipeline is arranged at the middle part of the oxidation tower and is connected with the outlet of the second strengthening reactor;
The condensation unit comprises a reaction kettle, a second built-in strengthening unit is arranged in the reaction kettle, and the second built-in strengthening unit is arranged at the top end of the reaction kettle.
In the prior art, the following problems mainly exist in the preparation of phenol acetone:
1. The reactor of the oxidation section adopts a typical bubbling reactor, and the size of the opening of the gas distributor is in millimeter level The size of the bubbles is larger, the bubbles are in millimeter-centimeter level generally, the bubbles are easy to be coalesced in the ascending process in the oxidation tower, the gas-liquid phase interface area is limited, and the mass transfer and reaction efficiency is low;
2. In the oxidation reaction process, as the concentration of Cumene Hydroperoxide (CHP) increases, the reaction temperature increases, the retention time of the CHP increases, and the side reaction products obviously increase;
3. The oxygen content in the gas phase at the top of the oxidation tower is high, the oxygen utilization rate is low, and the energy consumption is high.
In order to solve the technical problems, the utility model provides a phenol acetone preparation system which has a simple overall structure, and can crush and disperse reaction raw materials and oxygen into micron-sized bubbles by arranging a first built-in strengthening unit in a reaction tower, increase macroscopic reaction rate, improve mass transfer area between gas and liquid phases, prolong reaction time by arranging a pre-reaction pipeline at the middle part of an oxidation tower and connecting the pre-reaction pipeline with a second strengthening reactor, and perform reaction in the pre-reaction pipeline, so that cumene and oxygen can be primarily mixed, the phenomenon of aggregation of oxygen is avoided, and meanwhile, the utilization rate of oxygen is improved.
Preferably, a plurality of layers of baffle plates are sequentially arranged in the pre-reaction pipeline from top to bottom, and the baffle plates are arranged in a staggered manner;
Preferably, the baffle plate is arranged obliquely downwards along the direction away from the inner wall of the pre-reaction pipeline, and the inclination angle between the baffle plate and the side wall of the pre-reaction pipeline is 70-90 degrees. The baffle plates are arranged to prolong the residence time of the reaction raw materials in the pre-reaction pipeline, and break the vortex and the vortex in the pre-reaction pipeline through the baffle plates, so that the reaction raw materials and oxygen are more uniformly mixed in the pre-reaction pipeline, the problem of partial insufficient mixing or dead angle is reduced, and the mixing efficiency is improved; in addition, the baffle plates are arranged to improve the temperature distribution in the liquid, so that the heat transfer efficiency is improved; the angle between the baffle plate and the side wall of the pre-reaction pipeline is set to be 70-90 degrees, and the mixed shearing force can be reduced to a certain extent at 70-90 degrees, so that the reaction raw materials are stirred more gently, and byproducts are avoided.
Specifically, the number of the baffle plates is three, and the three baffle plates are distributed on the side wall of the pre-reaction pipeline at equal angles along the circumferential direction. The inclination angle of the uppermost baffle among the three baffles is 70 degrees, the inclination angle of the middle baffle is 80 degrees, and the inclination angle of the lowermost baffle is 90 degrees. The arrangement can lead the mixing effect to be increased in a gradient way, further prolong the flow path of the reaction raw materials, lead the baffle plate at the bottommost part to be vertical to the inner wall of the pre-reaction pipeline, effectively break vortex and improve the moderating effect.
Preferably, a third strengthening reactor is arranged at the bottom end of the oxidation tower, and the outlet of the third strengthening reactor is opposite to the outlet of the pre-reaction pipeline. By providing a third strengthening reactor opposite to the pre-reaction pipe outlet, hedging can be achieved.
Preferably, an inner coil is arranged on the inner wall of the oxidation tower, and the length of the inner coil is matched with the length of the pre-reaction pipeline. The reaction temperature can be regulated and controlled in an auxiliary way by arranging the inner coil pipe.
Specifically, the cooling water inlet of the inner coil is arranged above the cooling water outlet, so that the reaction temperature can be reduced.
Preferably, an external strengthening unit is arranged outside the oxidation tower and connected with the first internal strengthening unit, the external strengthening unit comprises a fourth strengthening reactor and a fifth strengthening reactor, and a communication pipeline is arranged between the fourth strengthening reactor and the fifth strengthening reactor. By arranging the external strengthening unit, the reaction raw materials and oxygen are crushed and dispersed before entering the reaction tower, so that the mass transfer area of a phase boundary is increased, and the reaction rate is improved.
In the utility model, a first built-in strengthening unit is arranged in an oxidation tower, the built-in strengthening unit is formed by combining a first strengthening reactor and a second strengthening reactor, and the two strengthening reactors are arranged in an up-down direction and are connected through a connecting pipe; the unreacted gas at the main tower top of the first strengthening reactor is sucked up, dispersed and crushed again and then returned to the second strengthening reactor through a connecting pipe for continuous reaction, so that the conversion rate of oxygen is improved; the second strengthening reactor is arranged below the first strengthening reactor and is connected with an external strengthening unit, reaction raw materials and oxygen which are introduced into the oxidation tower are subjected to secondary dispersion crushing, and the pressure energy of gas or the kinetic energy of circulating liquid which is conveyed into the oxidation tower is converted into bubble surface energy and is transmitted to the oxygen, so that micron-sized bubbles formed by crushing the oxygen react with the isopropylbenzene solution, the mass transfer area of gas-liquid two phases is increased, and the conversion rate and the utilization rate of the isopropylbenzene and the oxygen are increased; the micro bubbles of the first strengthening reactor can be dispersed again after entering the second strengthening reactor through the connecting pipe, so that the uniformity of the distribution of the micro bubbles in the liquid raw material is improved. In addition, the setting of connecting pipe can also play the supporting role to the second enhanced reactor, improves overall structure intensity.
The baffle plates are arranged in the pre-reaction pipeline in the oxidation tower, the baffle plates are multi-layered, preferably three-layered, and have a certain inclination angle, and the inclination angles of the three-layered baffle plates are sequentially increased, so that the residence time of the baffle plates in the pre-reaction pipeline can be prolonged, the vortex and vortex in the pre-reaction pipeline are broken through the inclined arrangement of the baffle plates, the reaction raw materials and oxygen are more uniformly mixed in the pre-reaction pipeline, and the problem of partial insufficient mixing or dead angles is solved.
The third strengthening reactor is arranged below the pre-reaction pipeline and connected with the oxygen inlet, and the third strengthening reactor is arranged in such a way that byproducts are generated in the cumene oxidation reaction process to inhibit the oxidation reaction, so that a small amount of oxygen is required to be introduced for many times to avoid the byproducts, and the conversion rate and the utilization rate of the oxygen can be improved.
The reaction kettle is internally provided with a second built-in strengthening unit which consists of a sixth strengthening reactor and a seventh strengthening reactor, wherein the two strengthening reactors are respectively arranged on opposite side walls in the reaction kettle, and the outlets of the two strengthening reactors are opposite, so that collision flow can be formed between the two strengthening reactors, and the dispersing effect is improved.
It will be appreciated by those skilled in the art that the enhanced reactors employed in the present utility model are described in the inventor's prior patents, such as patent application number CN201610641119.6、CN201610641251.7、CN201710766435.0、CN106187660、CN105903425A、CN109437390A、CN205833127U and CN 207581700U. The specific product structure and working principle of the micro bubble generator (i.e. the micro interface generator) are described in detail in the prior patent CN201610641119.6, and the application document describes that the micro bubble generator comprises a body and a secondary crushing member, the body is provided with a cavity, an inlet communicated with the cavity is arranged on the body, the opposite first end and the second end of the cavity are both open, wherein the cross-sectional area of the cavity is reduced from the middle part of the cavity to the first end and the second end of the cavity; the secondary crushing member is arranged at least one of the first end and the second end of the cavity, a part of the secondary crushing member is arranged in the cavity, and an annular channel is formed between the secondary crushing member and the through holes with two open ends of the cavity. The micro bubble generator also comprises an air inlet pipe and a liquid inlet pipe. The specific working principle of the structure disclosed in the application document is known as follows: the liquid enters the micro bubble generator tangentially through the liquid inlet pipe, and the gas is rotated and cut at ultrahigh speed to break the gas bubbles into micro bubbles in micron level, so that the mass transfer area between the liquid phase and the gas phase is increased, and the micro bubble generator in the patent belongs to a pneumatic micro interface generator.
In addition, in the prior patent 201610641251.7, it is described that the primary bubble breaker has a circulating liquid inlet, a circulating gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed inlet with the gas-liquid mixture outlet, which means that the bubble breaker needs to be mixed with gas and liquid, and in addition, as shown in the following figures, the primary bubble breaker mainly uses the circulating liquid as power, so that the primary bubble breaker belongs to a hydraulic micro-interface generator, and the secondary bubble breaker simultaneously introduces the gas-liquid mixture into an elliptical rotating ball for rotation, thereby realizing bubble breaking during rotation, so that the secondary bubble breaker actually belongs to a gas-liquid linkage micro-interface generator. In fact, both the hydraulic type micro-interface generator and the gas-liquid linkage type micro-interface generator belong to a specific form of the micro-interface generator, however, the micro-interface generator adopted by the utility model is not limited to the above-mentioned forms, and the specific structure of the bubble breaker described in the prior patent is only one form which can be adopted by the micro-interface generator of the utility model.
Furthermore, the prior patent 201710766435.0 states that the principle of the bubble breaker is that the high-speed jet flows are used for achieving the mutual collision of gases, and also states that the bubble breaker can be used for a micro-interface strengthening reactor, and verifies the relevance between the bubble breaker and the micro-interface generator; in addition, the prior patent CN106187660 also describes the specific structure of the bubble breaker, see paragraphs [0031] to [0041] in the specification, and the attached drawing details the specific working principle of the bubble breaker S-2, where the top of the bubble breaker is a liquid phase inlet, the side is a gas phase inlet, and the liquid phase entering from the top provides entrainment force, so as to achieve the effect of breaking into ultrafine bubbles, and in the attached drawing, the bubble breaker is in a cone-shaped structure, the diameter of the upper part is larger than that of the lower part, and the entrainment force can be better provided for the liquid phase.
Since the micro-interface generator was just developed in the early stage of the prior patent application, the micro-interface generator is named as a micro-bubble generator (CN 201610641119.6), a bubble breaker (201710766435.0) and the like in the early stage, and with the continuous technological improvement, the micro-interface generator is named as the later stage, and the reinforced reactor in the utility model is equivalent to the prior micro-bubble generator, the bubble breaker and the like, but the names are different. In summary, the enhanced reactor of the present utility model belongs to the prior art.
Preferably, the fourth strengthening reactor is connected with a cumene inlet, and the fifth strengthening reactor is connected with an oxygen inlet;
Preferably, an air filter is arranged between the oxygen inlet and the fifth strengthening reactor;
Preferably, the cumene inlet and the oxygen inlet are respectively connected with a regulating valve and a flowmeter. The feeding amounts of the cumene and the oxygen can be regulated and controlled by arranging the regulating valve and the flowmeter.
Preferably, a return pipeline is arranged outside the oxidation tower, an inlet of the return pipeline is connected with the side wall of the oxidation tower, and an outlet of the return pipeline is connected with the bottom of the oxidation tower;
Preferably, the return line is connected with a circulation cooler, which is connected with the return line inlet and the crude product outlet, respectively.
Preferably, a stirring paddle is arranged at the bottom end of the reaction kettle, a stirring paddle blade is connected to the stirring paddle, and the stirring paddle blade is arranged below the second built-in strengthening unit. The stirring paddle is arranged in the reaction kettle and matched with the second built-in strengthening unit to stir the microbubbles, so that the uniformity of dispersion of the microbubbles in the liquid in the reaction kettle is improved, and the reaction effect is further improved.
Preferably, a tail gas outlet is arranged at the top end of the reaction kettle, and the tail gas outlet is connected with the first strengthening reactor and the tail gas washing tower through gas pipelines respectively.
Compared with the prior art, the utility model has the beneficial effects that:
(1) According to the preparation system, the oxidation tower and the reaction kettle are arranged, and the first built-in strengthening unit and the second built-in strengthening unit are respectively arranged in the oxidation tower and the reaction kettle, so that the reaction efficiency and the conversion rate of raw materials are effectively improved;
(2) After the traditional bubbling reactor is changed into the strengthening technology, the mass transfer process of oxygen into the isopropylbenzene solution is strengthened, the macroscopic reaction rate is obviously increased, and the space-time yield of the oxidation tower is increased by 20% -30%; improves the oxidation reaction efficiency, shortens the reaction time and reduces the generation of byproducts.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the utility model. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
FIG. 1 is a schematic diagram of a system for preparing phenol acetone according to embodiment 1 of the present utility model;
Fig. 2 is a schematic structural diagram of a pre-reaction pipeline according to embodiment 1 of the present utility model.
Wherein:
a 1-oxidation column; 2-a first built-in reinforcement unit;
201-a first enhanced reactor; 202-a second enhanced reactor;
203-connecting the pipes; 3-pre-reaction pipeline;
301-baffle plate; 4-a third strengthening reactor;
5-an inner coil; 501-cooling water inlet;
502-a cooling water outlet; 6-an external strengthening unit;
601-fourth strengthening reactor; 602-a fifth enhanced reactor;
603-connecting a pipeline; 7-isopropylbenzene inlet;
8-oxygen inlet; 9-an air filter;
10-regulating valve; 11-a flow meter;
12-a return line; 121-a circulation cooler;
13-a reaction kettle; 14-a second built-in reinforcement unit;
141-sixth enhanced reactor; 142-seventh enhanced reactor;
15-stirring paddles; 151-stirring blades;
16-a tail gas outlet; 17-gas line;
18-a tail gas washing tower; 19-oxygen tank.
Detailed Description
The technical solution of the present utility model will be clearly and completely described below with reference to the accompanying drawings and detailed description, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present utility model, and are intended to be illustrative of the present utility model only and should not be construed as limiting the scope of the present utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In the description of the present utility model, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
In order to more clearly illustrate the technical scheme of the utility model, the following description is given by way of specific examples.
Example 1
Referring to fig. 1-2, the system for preparing phenol acetone according to the embodiment of the utility model comprises an oxidation unit and a condensation unit which are sequentially connected;
The oxidation unit comprises an oxidation tower 1, a first built-in strengthening unit 2 is arranged in the oxidation tower 1, the first built-in strengthening unit 2 is arranged at the top end of the oxidation tower 1, the first built-in strengthening unit 2 comprises a first strengthening reactor 201 and a second strengthening reactor 202, the first strengthening reactor 201 is arranged above the second strengthening reactor 202, a connecting pipe 203 is arranged between the first strengthening reactor 201 and the second strengthening reactor 202, and the first strengthening reactor 201 is arranged above the liquid level; the outside of the oxidation tower 1 is provided with an external strengthening unit 6, the external strengthening unit 6 comprises a fourth strengthening reactor 601 and a fifth strengthening reactor 602, the fourth strengthening reactor 601 is arranged above the fifth strengthening reactor 602, a communication pipeline 603 is arranged between the fourth strengthening reactor 601 and the fifth strengthening reactor 602, specifically, the fourth strengthening reactor 601 is connected with a cumene inlet 7, the fifth strengthening reactor 602 is connected with an oxygen inlet 8, and the second strengthening reactor 202 is connected with the external strengthening unit 6. After the cumene liquid and the oxygen are dispersed and crushed into micron-sized bubbles in the external strengthening unit 6, the micron-sized bubbles enter the oxidation tower 1, and are secondarily crushed and dispersed through the second strengthening reactor 202, so that the phase boundary mass transfer area between the gas phase and the liquid phase is increased.
In order to accurately control the reaction system, the cumene inlet 7 and the oxygen inlet 8 are respectively connected with a regulating valve 10 and a flowmeter 11, so that the feeding amounts of cumene liquid and oxygen can be regulated and controlled.
To ensure the purity of the produced phenol acetone, an air filter 9 is provided between the oxygen inlet 8 and the fifth strengthening reactor 602 to ensure the purity of the oxygen entering the oxidation column 1.
In this embodiment, the first strengthening reactor 201 is located at the top of the oxidation tower 1, and the first strengthening reactor 201 is located above the liquid level in the oxidation tower 1, and the gas above the liquid level in the oxidation tower 1 enters the first strengthening reactor 201 through the gas pipeline 17. During the reaction, unreacted gas above the liquid level of the oxidation tower 1 is sucked into the first strengthening reactor 201 through the gas pipeline 17, dispersed and crushed by the first strengthening reactor 201 and returned into the oxidation tower 1 for continuous reaction, so that the conversion rate of oxygen is improved.
The middle part of the oxidation tower 1 is provided with a pre-reaction pipeline 3, the pre-reaction pipeline 3 is connected with the outlet of the second strengthening reactor 202, the bottom end of the oxidation tower 1 is provided with a third strengthening reactor 4, the third strengthening reactor 4 is connected with an oxygen inlet 8, and the outlet of the third strengthening reactor 4 is opposite to the outlet of the pre-reaction pipeline 3, so that the reaction in the pre-reaction pipeline 3 and the oxygen microbubbles at the outlet of the third strengthening reactor 4 can be opposite to each other, and the effects of stirring reaction raw materials and improving the reaction rate are achieved.
With continued reference to fig. 2, the inside of the pre-reaction pipeline 3 is sequentially provided with a plurality of baffle plates 301 from top to bottom, and the baffle plates 301 are staggered; specifically, the baffle plate 301 is arranged obliquely downwards along the direction away from the inner wall of the pre-reaction pipeline 3, and the inclination angle between the baffle plate 301 and the side wall of the pre-reaction pipeline 3 is 70-90 degrees.
Specifically, in this embodiment, the number of baffles 301 is three, the three baffles 301 are equiangularly distributed on the outer wall of the pre-reaction tube 3 in the circumferential direction, the angle of inclination of the uppermost baffle 301 among the three baffles 301 is 70 °, the angle of inclination of the middle baffle 301 is 80 °, and the angle of inclination of the lowermost baffle 301 is 90 °. The arrangement can increase the mixing effect in a gradient manner, further prolong the flow path of the reaction raw materials, and lead the baffle plate 301 at the bottommost part to be vertical to the inner wall of the pre-reaction pipeline 3, thereby effectively breaking vortex and improving the moderating effect.
In order to improve the radiating effect of the oxidation tower 1, an inner coil 5 is arranged on the inner wall of the oxidation tower 1, the length of the inner coil 5 is matched with the length of the pre-reaction pipeline 3, a cooling water inlet 501 of the inner coil 5 is arranged above a cooling water outlet 502, and the reaction temperature can be regulated and controlled in an auxiliary manner by arranging the inner coil 5.
In the embodiment of the utility model, the bottom end of the oxidation tower 1 is also provided with the third strengthening reactor 4, and the outlet of the third strengthening reactor 4 is opposite to the outlet of the pre-reaction pipeline 3, so that the mixed solution generated by the primary reaction in the pre-reaction pipeline 3 can realize opposite flushing with oxygen from the third strengthening reactor 4, thereby stirring the gas-liquid mixture in the oxidation tower 1.
With continued reference to fig. 1, a return pipeline 12 is arranged outside the oxidation tower 1, an inlet of the return pipeline 12 is connected with the side wall of the oxidation tower 1, and an outlet of the return pipeline 12 is connected with the bottom of the oxidation tower 1; the return line 12 is connected to a circulation cooler 121, and the circulation cooler 121 is connected to an inlet of the return line 12 and an outlet of the crude product, respectively.
The condensation unit is connected with the oxidation unit, and specifically, the reaction kettle 13 of the condensation unit is connected with the crude product outlet of the oxidation unit and is used for carrying out condensation reaction on the phenol and acetone mixed solution.
Specifically, a second built-in strengthening unit 14 is disposed in the reaction kettle 13, the second built-in strengthening unit 14 is disposed at the top end of the reaction kettle 13, the second strengthening unit includes a sixth strengthening reactor 141 and a seventh strengthening reactor 142, the two strengthening reactors are disposed on opposite side walls in the reaction kettle 13 and opposite in outlet, so that collision flow can be formed between the two strengthening reactors, and dispersion effect is improved. Specifically, the sixth enhanced reactor 141 is connected to the crude product outlet, and the seventh enhanced reactor 142 is connected to the oxygen tank 19.
In this embodiment, a stirring paddle 15 is disposed at the bottom end of the reaction kettle 13, a stirring paddle 151 is connected to the stirring paddle 15, and the stirring paddle 151 is disposed below the second built-in reinforcement unit 14. The stirring paddle 15 is arranged in the reaction kettle 13 and matched with the second built-in strengthening unit 14, so that the micro-bubbles coming out of the sixth strengthening reactor 141 and the seventh strengthening reactor 142 are stirred, the dispersion uniformity of the micro-bubbles in the liquid in the reaction kettle 13 is improved, and the reaction effect is further improved.
The preparation method of the preparation system of the embodiment is as follows: the cumene and the oxygen are mixed in the oxidation tower 1 after being dispersed and crushed into micro-bubbles in micron order to generate a phenol and acetone crude solution, the phenol and acetone crude solution enters the reaction kettle 13, and the oxygen reacts with the crude product through the seventh strengthening reactor 142 to obtain a phenol and acetone solution.
Example 2
The difference between this example and example 1 is only that the baffles in the pre-reaction tube are all inclined at 80 °.
Example 3
The difference between this example and example 1 is only that the pre-reaction pipes are all inclined at 45 °.
Example 4
The present example differs from example 1 only in that the third strengthening reactor is not provided.
Comparative example 1
The difference between this example and example 1 is only that no baffles are provided in the pre-reaction tube.
Comparative example 2
The present example differs from example 1 only in that no pre-reaction tube was provided.
Comparative example 3
The present example differs from embodiment 1 only in that the first built-in reinforcement unit is not provided.
Comparative example 4
In the method, the prior art is adopted, cumene liquid is directly introduced into the bottom of an oxidation tower, fresh air which is sent by a compressor and subjected to alkali washing is introduced into the bottom of the oxidation tower, reaction is carried out in the oxidation tower to generate a reaction product, and the reaction product enters an enterprise separation tank for separation and then enters a subsequent concentration section.
Experimental example 1
Phenol acetone was prepared by using the preparation systems of examples 1 to 4 and comparative examples 1 to 3, respectively, and the specific experimental conditions were as follows: the mass flow rate of the isopropylbenzene is 3003.2kg/h, the volume flow rate of the isopropylbenzene is 3.7m 3/h, the mass flow rate of the oxygen is 573.0kg/h, and the volume flow rate of the oxygen is 96.1m 3/h. The reaction results are shown in the following table:
table 1 experimental results
When the prior art is used for preparing the phenol acetone, the selectivity of CHP is generally about 60.56%, the tail oxygen content is 5.1%, the oxygen utilization rate is 69%, and the yield of the phenol acetone is 62%. As can be seen from Table 1, compared with the existing oxidation tower, the phenol acetone yield of each embodiment of the utility model is obviously increased, the phenol acetone yield of the embodiment 1 is increased by 36%, the oxygen content of the tail gas of the reaction system of each embodiment of the utility model is lower than 5%, the oxygen content of the tail gas of each embodiment of the utility model is reduced by 0.8-4% compared with the prior art, and the reaction time and the reaction temperature of each embodiment of the utility model are lower than those of the prior art.
As can be seen from table 1, the reaction temperature of the preparation system of the present utility model is obviously lower than that of the reaction temperature of the preparation of phenol acetone in the prior art, and the reaction time is obviously shortened, so that the preparation system still has good raw material conversion rate and product yield, and simultaneously the CHP selectivity is obviously improved, which indicates that the baffle arrangement mode and the strengthening reactor arrangement mode of the embodiment 1 can achieve the optimal reaction effect, and therefore, the preparation system of the present utility model has low reaction energy consumption and good preparation effect.
The phenol acetone yield of comparative example 3 was lower than that of example 1 because comparative example 3 was not provided with the first built-in reinforcing unit, which could not sufficiently break and disperse cumene and oxygen in the oxidation tower, and could not realize the opposite flushing with the third reinforcing reactor, and it can be seen that this example improved the phenol acetone yield by setting the arrangement of the reinforcing reactors of the oxidation tower.
In a word, compared with the prior art, the preparation system of the phenol acetone has the advantages of easy realization of reaction temperature, short reaction time, high raw material conversion rate and high product yield, and is worthy of wide popularization and application.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present utility model, and not for limiting the same; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the utility model.
Claims (9)
1. A system for preparing phenol-acetone, comprising:
the oxidation unit comprises an oxidation tower, a first built-in strengthening unit is arranged in the oxidation tower, and the first built-in strengthening unit is arranged at the top end of the oxidation tower;
The first built-in strengthening unit comprises a first strengthening reactor and a second strengthening reactor, the first strengthening reactor is arranged above the second strengthening reactor, a connecting pipe is arranged between the first strengthening reactor and the second strengthening reactor, and the first strengthening reactor is arranged above the liquid level;
A pre-reaction pipeline is arranged at the middle part of the oxidation tower and is connected with the outlet of the second strengthening reactor;
The condensation unit comprises a reaction kettle, a second built-in strengthening unit is arranged in the reaction kettle, and the second built-in strengthening unit is arranged at the top end of the reaction kettle.
2. The system for preparing phenol acetone according to claim 1, wherein a plurality of layers of baffle plates are sequentially arranged in the pre-reaction pipeline from top to bottom, and the baffle plates are arranged in a staggered manner;
The baffle plate is arranged obliquely downwards along the direction away from the inner wall of the pre-reaction pipeline, and the inclination angle between the baffle plate and the side wall of the pre-reaction pipeline is 70-90 degrees.
3. The system for preparing phenol acetone according to claim 1, wherein a third strengthening reactor is arranged at the bottom end of the oxidation tower, and the outlet of the third strengthening reactor is opposite to the outlet of the pre-reaction pipeline.
4. The system for preparing phenol acetone according to claim 1, wherein the inner wall of the oxidation tower is provided with an inner coil, the length of which is adapted to the length of the pre-reaction pipe.
5. The phenol acetone preparation system of claim 1, wherein an external strengthening unit is arranged outside the oxidation tower, the external strengthening unit is connected with the first internal strengthening unit, the external strengthening unit comprises a fourth strengthening reactor and a fifth strengthening reactor, and a communication pipeline is arranged between the fourth strengthening reactor and the fifth strengthening reactor.
6. The system for preparing phenol acetone according to claim 5, wherein the fourth strengthening reactor is connected to a cumene inlet, and the fifth strengthening reactor is connected to an oxygen inlet;
an air filter is arranged between the oxygen inlet and the fifth strengthening reactor;
the cumene inlet and the oxygen inlet are respectively connected with a regulating valve and a flowmeter.
7. The system for preparing phenol acetone according to claim 1, wherein a reflux pipeline is arranged outside the oxidation tower, an inlet of the reflux pipeline is connected with the side wall of the oxidation tower, and an outlet of the reflux pipeline is connected with the bottom of the oxidation tower;
The return line is connected with a circulation cooler, and the circulation cooler is respectively connected with a return line inlet and a crude product outlet.
8. The phenol acetone preparation system according to claim 1, wherein a stirring paddle is arranged at the bottom end of the reaction kettle, a stirring paddle blade is connected to the stirring paddle blade, and the stirring paddle blade is arranged below the second built-in strengthening unit.
9. The system for preparing phenol acetone according to claim 1, wherein a tail gas outlet is arranged at the top end of the reaction kettle, and the tail gas outlet is connected with the first strengthening reactor and the tail gas washing tower through gas pipelines respectively.
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