A device for continuously producing aromatic ketones and a method for using the same

Abstract

The invention discloses a device for continuously producing aromatic ketone in the technical field of aromatic ketone production and a method for using the device. The device comprises a raw material tank, a metering pump, a tubular reactor, a heating device, a receiving tank and an absorption tank. The liquid inlet end of the tubular reactor is connected with the raw material tank through the metering pump, and the liquid outlet end is connected with the receiving tank. The heating device is fixedly installed on the surface of the tubular reactor. The air inlet end of the second separator is connected with the receiving tank through the second condenser, and the air inlet end of the absorption tank is connected with the air outlet end of the second separator. The upper side of the middle of the tubular reactor is connected with a plurality of first condensers at the same interval, and the air outlet end of each first condenser is connected with the first separator. The invention uses a tubular reactor, can produce continuously, has a short residence time of materials in the reactor, has few side reactions, has a high product yield, greatly improves the safety of industrial production, and is easy to realize automatic control.

Description

Technical Field

[0001] The invention relates to the technical field of aromatic ketone production, in particular to a device for continuously producing aromatic ketone and a use method thereof. Background Art

[0002] Aromatic ketones refer to aromatic compounds containing carbonyl groups. A compound in which two single bonds on the carbonyl group are connected to two hydrocarbon groups is a ketone, with a simplified structural formula of R-CO-R. A pure aromatic ketone is one in which both hydrocarbon groups are aromatic, with a simplified structural formula of Ar-CO-Ar'. A mixed aromatic ketone is one in which only one hydrocarbon group is aromatic, with a simplified structural formula of Ar-CO-R.

[0003] Aromatic ketones such as benzophenone and p-chlorobenzophenone are widely used in the fields of cosmetics, fragrances, dyes, medicines, UV radiation curing, etc. There are many ways to synthesize aromatic ketones, and the most common one is the reaction of aromatic hydrocarbons or halogenated aromatic hydrocarbons with aromatic acid chlorides under the catalysis of metal chlorides. Using this synthesis route, the current industrial production method usually uses a reactor as the main reaction equipment, and the reaction is carried out intermittently under high temperature and high pressure. The reactor is used as a reaction container for raw materials, and the reaction time is long, the equipment liquid holding capacity is large, and the equipment utilization rate and production efficiency are low. More importantly, there are certain safety risks.

[0004] Based on this, the present invention designs a device for continuously producing aromatic ketone and a method for using the device to solve the above problems. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a device for continuously producing aromatic ketones and a method for using the device. The device has the characteristics of continuous production, high production efficiency, easy automatic control and intrinsically safe production.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A device for continuously producing aromatic ketones comprises a raw material tank, a metering pump, a tubular reactor, a heating device, a first condenser, a first separator, a receiving tank, an absorption tank, a second condenser and a second separator. The liquid inlet end of the tubular reactor is connected to the raw material tank through the metering pump, and the liquid outlet end is connected to the receiving tank. The heating device is fixedly installed on the surface of the tubular reactor. The air inlet end of the second separator is connected to the receiving tank through the second condenser. The air inlet end of the absorption tank is connected to the air outlet end of the second separator. The upper side of the middle part of the tubular reactor is connected to a plurality of first condensers at the same interval. The air outlet end of each first condenser is connected to the first separator, and the air outlet ends of the plurality of first separators are connected to the second condenser through an exhaust pipe.

[0008] In the device for continuously producing aromatic ketone as described above, a back pressure valve is further provided between the tubular reactor and the receiving tank, and an exhaust valve is provided on the surface of the tubular reactor.

[0009] In the device for continuously producing aromatic ketones as described above, the tubular reactor is further in a continuous bending shape, preferably a continuous U-shape, having a plurality of upper and lower bends.

[0010] The device for continuously producing aromatic ketones as described above of the present invention, further, the first condenser includes an eccentric tee, the two ends of the bottom of the eccentric tee are connected to the upper bend of the tubular reactor, the top of the eccentric tee is connected to a buffer, the upper part of the buffer is fixedly connected to a condensation shell, the inner cavity of the condensation shell is fixedly connected to a condensation coil, one end of the condensation coil is connected to the buffer, and the other end passes through the outside of the condensation shell and is connected to the first separator, the lower end of the side of the condensation shell is provided with a cooling water inlet, and the upper part is provided with a cooling water outlet, the bottom end of the first separator is connected to the buffer through a U-shaped tube, and the bottom of the buffer is fixedly connected to a demister located at the bottom of the liquid outlet end of the U-shaped tube.

[0011] In the device for continuously producing aromatic ketone as described above, the heating device is further a steam heater, a thermal oil heater or an electric heater, preferably an electric heater, and further an electric heater.

[0012] The device for continuously producing aromatic ketones of the present invention is as described above. Further, the reaction temperature in the tubular reactor is set and controlled in sections using an electric heater to ensure the activity of the catalyst and the rapid and complete synthesis reaction, and the temperature in the rear section of the tubular reactor is higher than the temperature in the front section.

[0013] The device for continuously producing aromatic ketone of the present invention is as described above, further, a filter is arranged between the raw material tank and the metering pump.

[0014] The device for continuously producing aromatic ketone of the present invention as described above, further, flow meters are arranged between the metering pump and the tubular reactor, between the first separator and the exhaust pipe, and between the absorption tank and the second separator, and a liquid level meter is arranged between the first condenser and the tubular reactor.

[0015] The device for continuously producing aromatic ketone of the present invention is as described above, further, the surface of the tubular reactor is also provided with a thermometer and a pressure gauge, and observation mirrors are provided between the first separator and the exhaust pipe and on the surface of the tubular reactor.

[0016] The device for continuously producing aromatic ketone of the present invention is as described above, further, the lower bend of each tubular reactor is provided with a sampling port.

[0017] The device for continuously producing aromatic ketone of the present invention as described above, further, the lower bends of the plurality of tubular reactors are connected to an emergency pipeline, and a safety valve is provided on the emergency pipeline.

[0018] The present invention also provides a method for using the above-mentioned device for continuously producing aromatic ketones. When producing aromatic ketones, the reaction liquid is stored in a raw material tank. First, the heating device is turned on to heat each section of the tubular reactor to a set temperature, and then the metering pump is turned on to extract the reaction liquid in the raw material tank. The reaction liquid enters the tubular reactor through the metering pump. The gas generated by the reaction enters the absorption tank through the first condenser and the second condenser, the first separator and the second separator, and the exhaust pipe to be absorbed by water. The entrained liquid material is returned to the tubular reactor and the receiving tank respectively through the first separator and the second separator. The material after the reaction is completely entered into the receiving tank.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: the present invention uses a tubular reactor, the reaction liquid for producing aromatic ketone is pumped from a reaction tank into the tubular reactor by a metering pump, the tubular reactor is heated by a heating device, the reaction liquid reacts while flowing in the tubular reactor, the gas generated by the reaction is cooled and separated by a condenser and a separator, the gas is absorbed by an absorption tank, and the material after the reaction is completely reacted enters a receiving tank, thereby enabling continuous production, the material stays in the reactor for a short time, there are few side reactions, the product yield reaches 95%, the safety of industrial production is greatly improved, and automatic control is easy to achieve.

[0020] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to explain the present invention more clearly, the technical solutions of the embodiments will be described below. By briefly introducing the drawings required for use, the inherent advantages and unique features of the present invention can be clearly seen. It should be pointed out that the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, it is easy to obtain other drawings based on these drawings without creative work.

[0022] Figure 1 It is a structural schematic diagram of the present invention;

[0023] Figure 2 for Figure 1 The enlarged schematic diagram of point A in the middle;

[0024] Figure 3 for Figure 1 The enlarged schematic diagram of point B in the middle;

[0025] Figure 4It is a cross-sectional schematic diagram of the connection structure between the first condenser and the first separator of the present invention;

[0026] Figure 5 is a three-dimensional schematic diagram of the condensing coil of the present invention;

[0027] In the accompanying drawings, the components represented by the reference numerals are listed as follows:

[0028] 1-raw material tank, 2-filter, 3-metering pump, 4-flow meter, 5-tubular reactor, 6-heating device, 7-observation mirror, 8-first condenser, 81-eccentric tee, 82-buffer, 83-condensation shell, 84-condensation coil, 85-cooling water inlet, 86-cooling water outlet, 87-U-tube, 88-demister, 9-first separator, 10-sampling port, 11-receiving tank, 12-absorption tank, 13-second condenser, 14-second separator, 15-liquid level meter, 16-back pressure valve, 17-emergency pipeline, 18-pressure gauge, 19-exhaust pipeline, 20-thermometer. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] See also Figure 1-5The present invention provides a technical solution: a device for continuously producing aromatic ketones, comprising a raw material tank 1, a filter 2, a metering pump 3, a flow meter 4, a tubular reactor 5, a heating device 6, an observation mirror 7, a first condenser 8, a first separator 9, a sampling port 10, a receiving tank 11, an absorption tank 12, a second condenser 13, a second separator 14, a liquid level meter 15, a back pressure valve 16, an emergency pipeline 17, a pressure gauge 18, an exhaust pipeline 19 and a thermometer 20, wherein the raw material tank 1 is used to store a uniformly mixed reaction liquid, the tubular reactor 5 is in a continuous U-shape, and has five upper bends and six lower bends, the liquid inlet end of the tubular reactor 5 is connected to the raw material tank 1 through the metering pump 3, and the liquid outlet end is connected to the receiving tank 11, the receiving tank 11 is provided with two groups, and the two groups of receiving tanks 11 are connected, the reaction liquid in the raw material tank 1 is pumped into the tubular reactor 5 by the metering pump 3, and the flow rate of the reaction liquid can be controlled; the raw material tank 1 and the metering pump 3 is provided with a filter 2, and when the reaction liquid passes through the filter 2, the filter 2 can filter out solid impurities in the reaction liquid; a back pressure valve 16 is provided between the tubular reactor 5 and the receiving tank 11, and an exhaust valve is provided on the surface of the tubular reactor 5. The pressure in the pipeline and the outflow speed of the reaction materials are controlled by adjusting the back pressure valve 16 and the exhaust valve to ensure that the reaction liquid has enough reaction time in the tubular reactor 5; a sampling port 10 is provided at the lower bend of each tubular reactor 5. The user can open the sampling port 10, take out the sample from the tubular reactor 5 and test it, so as to obtain the reaction degree of the reaction liquid in each section of the tubular reactor 5; the lower bends of the six tubular reactors 5 are connected with an emergency pipeline 17, and a safety valve is provided on the emergency pipeline 17. In case of an accident, the reaction liquid in the tubular reactor 5 can be discharged through the emergency pipeline 17, which provides additional safety protection for the device and further improves the safety of the device;

[0031] The heating device 6 is fixedly mounted on the surface of the tubular reactor 5. The heating device 6 is an electric heater, which includes an insulation layer, a heating coil, a temperature probe and a control cabinet arranged outside the tubular reactor 5. The reaction temperature in the tubular reactor 5 is set and controlled in sections using an electric heater to ensure the activity of the catalyst and the rapid and complete synthesis reaction. The temperature in the rear section of the tubular reactor 5 is higher than the temperature in the front section, preferably 10-50°C higher, so that the reaction liquid in the tubular reactor 5 can react more fully. The air inlet end of the second separator 14 is connected to the receiving tank 11 through the second condenser 13, and the air inlet end of the absorption tank 12 is connected to the outlet end of the second separator 14. The first condenser 8 is connected to the gas end, and two groups of absorption tanks 12 are provided, and the two groups of absorption tanks 12 are connected. The top of the upper bend of the tubular reactor 5 is connected to the first condenser 8, and the gas outlet end of each first condenser 8 is connected to the first separator 9. The gas outlet ends of the five first separators 9 are connected to the second condenser 13 through the exhaust pipe 19. The first condenser 8 and the second condenser 13 are both used to cool the gas and the material entrained by the gas. The first separator 9 and the second separator 14 are both used to separate the gas produced by the reaction from the material. Among them, the first condenser 8 cools the gas produced by the reaction liquid in the tubular reactor 5 during the reaction and the material entrained by the gas. , allowing the material to flow back to the tubular reactor 5, the first separator 9 performs gas-liquid separation on the gas flowing out of the first condenser 8, allowing the liquid to flow back to the first condenser 8, the second condenser 13 cools the gas produced by the generated liquid in the receiving tank 11 and the material entrained in the gas, allowing the material to flow back to the receiving tank 11, the second separator 14 performs gas-liquid separation on the gas flowing out of the second condenser 13, allowing the liquid to flow back to the second condenser 13, in addition, flow meters 4 are provided between the metering pump 3 and the tubular reactor 5, between the first separator 9 and the exhaust pipe 19, and between the absorption tank 12 and the second separator 14, through the flow meter 4 displays the actual flow rate of the reaction liquid and the escape flow rate of the gas. A liquid level gauge 15 is arranged between the first condenser 8 and the tubular reactor 5, so as to conveniently observe the rising height of the material in the tubular reactor 5 during gas-liquid separation. A thermometer 20 and a pressure gauge 18 are also arranged near the upper bend of the tubular reactor 5. The reaction temperature of each section of the tubular reactor 5 can be monitored by the thermometer 20, and the reaction pressure of each section of the tubular reactor 5 can be monitored by the pressure gauge 18. Observation mirrors 7 are arranged between the first separator 9 and the exhaust pipe 19 and on the surface of the tubular reactor 5, so as to conveniently observe the reaction state of the material and the state of gas and liquid in the tubular reactor 5.

[0032] Specifically, the structure of the first condenser 8 is as follows: Figure 4 and Figure 5As shown: the first condenser 8 includes an eccentric three-way pipe 81, the two ends of the bottom of the eccentric three-way pipe 81 are connected to the upper bend of the tubular reactor 5, the top of the eccentric three-way pipe 81 is connected to a buffer 82, the upper part of the buffer 82 is fixedly connected to a condensation shell 83, the condensation shell 83 is a fully enclosed shell, the inner cavity of the condensation shell 83 is fixedly connected to a condensation coil 84, one end of the condensation coil 84 is connected to the buffer 82, and the other end passes through the outside of the condensation shell 83 and is connected to the first separator 9, the lower end of the side of the condensation shell 83 is provided with a cooling water inlet 85, and the upper part is provided with a cooling water outlet 86, the bottom end of the first separator 9 is connected to the buffer 82 through a U-shaped tube 87, and the bottom of the buffer 82 is fixedly connected to a defoamer 88 located at the bottom of the liquid outlet end of the U-shaped tube 87. When working, the inner cavity of the condensation shell 83 has cooling water flowing upward, and the reaction liquid in the tubular reactor 5 flows from right to left in the horizontal part of the eccentric three-way pipe 81. The gas generated by the reaction enters the condensation coil 84 through the buffer 82. The gas in the condensation coil 84 and the entrained material are cooled by cooling water to condense the material into a liquid state. A part of the liquid material flows downward from the vertical section of the condensation coil 84 into the buffer 82, and the other part of the liquid material flows into the first separator 9 along the outer spiral section of the condensation coil 84, and then flows downward from the first separator 9 through the U-shaped tube 87 into the buffer 82, and finally flows back to the tubular reactor 5. Among them, the setting of the buffer 82 increases the height of the condensation shell 83, which effectively prevents the reaction liquid in the tubular reactor 5 from rushing into the condensation coil 84 under the action of the upward flow of gas. The setting of the demister 88 can prevent the loss of useful products or contamination of the condensed liquid. The setting of the U-shaped tube 87 allows the U-shaped tube 87 to have a sealing liquid to prevent the gas from directly flowing into the first separator 9.

[0033] It should be noted that: in this embodiment, the components can be connected through connecting pipes, and corresponding control valves are provided on the connecting pipes.

[0034] The method of using the above-mentioned device for continuously producing aromatic ketones is as follows: when producing aromatic ketones, the reaction liquid is stored in the raw material tank 1, and the various sections of the tubular reactor 5 are first heated to the set temperature by turning on the heating device 6, and then the metering pump 3 is turned on to extract the reaction liquid in the raw material tank 1. The reaction liquid enters the tubular reactor 5 through the filter 2 and the metering pump 3 in sequence, and the gas generated by the reaction enters the absorption tank 12 through the first condenser 8 and the second condenser 13, the first separator 9 and the second separator 14, and the exhaust pipe 19 to be absorbed by water. The entrained liquid material is returned to the tubular reactor 5 and the receiving tank 11 respectively through the first separator 9 and the second separator 14, and the material after the reaction is completely entered into the receiving tank 11.

[0035] Specifically, 150 kg of benzene (1923 mol), 1 kg of anhydrous ferric chloride (6.15 mol) and 70 kg of benzoyl chloride (500 mol) were mixed to form a reaction liquid, which was placed in a raw material tank 1. An electric heater was used to control the temperature in a tubular reactor 5 in three stages according to the direction of liquid flow, and the temperature was controlled at 150° C., 180° C. and 220° C. respectively. The reaction liquid flowing out of the outlet of the raw material tank 1 was pumped into the tubular reactor 5 by a metering pump 3. The volume of the tubular reactor 5 was 100 L. The flow rate of the metering pump 3 was controlled, and the back pressure valve 16 and the exhaust valve were used to control the flow rate of the tubular reactor 5. The reaction pressure in the tubular reactor 5 is 1.5 MPa, so that the flow rate of the reaction liquid in the tubular reactor 5 is 60 L / h. The liquid material after the reaction discharged from the outlet of the tubular reactor 5 enters the receiving tank 11. The gas generated by the reaction passes through the first condenser 8 and the second condenser 13, the first separator 9 and the second separator 14, and the matching exhaust pipe 19, and enters the absorption tank 12 to be absorbed by water. The entrained liquid material returns to the tubular reactor 5 and the receiving tank 11 respectively through the first separator 9 and the second separator 14. The material after the reaction is completely entered into the receiving tank 11.

[0036] During the production process, the back pressure valve 16 and the exhaust valve are used to control the total pressure of the pipeline and the outflow rate of the reaction materials. The temperature, pressure and gas separation conditions of each section of the tubular reactor 5 are observed and monitored through the thermometers 20, the pressure gauges 18 and the flowmeter 4. The reaction degree of the materials in each section of the tubular reactor 5 is judged by the samples obtained at each sampling port 10. The movement state of the materials is observed through the observation mirror 7. The material feed rate is adjusted by the observation mirror 7. The reaction temperature of the reaction liquid in the tubular reactor 5 is set by the heating device 6. The pressure in the reaction tubular reactor 5 is adjusted by the back pressure valve 16 and the exhaust valve. The reaction endpoint of the last sampling point sample is when the raw material acyl chloride basically disappears.

[0037] The electrical components mentioned in this article are all connected to an external main controller and 220V mains electricity, and the main controller can be a conventional known device for controlling a computer or the like.

[0038] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0039] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A device for continuously producing aromatic ketones, characterized in that: The invention comprises a raw material tank (1), a metering pump (3), a tubular reactor (5), a heating device (6), a first condenser (8), a first separator (9), a receiving tank (11), an absorption tank (12), a second condenser (13) and a second separator (14); the liquid inlet end of the tubular reactor (5) is connected to the raw material tank (1) through the metering pump (3), and the liquid outlet end is connected to the receiving tank (11); two groups of receiving tanks (11) are provided, and the two groups of receiving tanks (11) are connected; the heating device (6) is fixedly mounted on The surface of the tubular reactor (5), the gas inlet end of the second separator (14) is connected to the receiving tank (11) through the second condenser (13), the gas inlet end of the absorption tank (12) is connected to the gas outlet end of the second separator (14), the upper side of the middle part of the tubular reactor (5) is connected to a plurality of first condensers (8) at the same intervals, the gas outlet end of each first condenser (8) is connected to the first separator (9), and the gas outlet ends of the plurality of first separators (9) are connected to the second condenser (13) through an exhaust pipe (19); The first condenser (8) comprises an eccentric three-way pipe (81), the two ends of the bottom of the eccentric three-way pipe (81) are connected to the upper bend of the tubular reactor (5), the top of the eccentric three-way pipe (81) is connected to a buffer (82), the upper part of the buffer (82) is fixedly connected to a condensation shell (83), the inner cavity of the condensation shell (83) is fixedly connected to a condensation coil (84), one end of the condensation coil (84) is connected to the buffer (82), and the other end passes through the outside of the condensation shell (83) and is connected to the first separator (9), the lower end of the side of the condensation shell (83) is provided with a cooling water inlet (85), and the upper part is provided with a cooling water outlet (86), the bottom end of the first separator (9) is connected to the buffer (82) through a U-shaped pipe (87), and the bottom of the buffer (82) is fixedly connected to a defoamer (88) located at the bottom of the liquid outlet end of the U-shaped pipe (87); The heating device (6) is a steam heater, a thermal oil heater or an electric heater; The reaction temperature in the tubular reactor (5) is set and controlled in sections using an electric heater, and the temperature in the rear section of the tubular reactor (5) is higher than the temperature in the front section.

2. The device for continuously producing aromatic ketone according to claim 1, characterized in that: A back pressure valve (16) is provided between the tubular reactor (5) and the receiving tank (11), and an exhaust valve is provided on the surface of the tubular reactor (5).

3. The device for continuously producing aromatic ketone according to claim 2, characterized in that: The tubular reactor (5) is in a continuously bent shape, having a plurality of upper bends and lower bends.

4. The device for continuously producing aromatic ketone according to claim 1, characterized in that: A flow meter (4) is provided between the metering pump (3) and the tubular reactor (5), between the first separator (9) and the exhaust pipe (19), and between the absorption tank (12) and the second separator (14), and a liquid level meter (15) is provided between the first condenser (8) and the tubular reactor (5).

5. The device for continuously producing aromatic ketone according to claim 4, characterized in that: A filter (2) is provided between the raw material tank (1) and the metering pump (3), a thermometer (20) and a pressure gauge (18) are also provided on the surface of the tubular reactor (5), and an observation mirror (7) is provided between the first separator (9) and the exhaust pipe (19) and on the surface of the tubular reactor (5).

6. The device for continuously producing aromatic ketone according to claim 5, characterized in that: The lower bend of each tubular reactor (5) is provided with a sampling port (10), the lower bends of the plurality of tubular reactors (5) are connected to an emergency pipeline (17), and a safety valve is provided on the emergency pipeline (17).

7. A method for using the device for continuously producing aromatic ketone according to any one of claims 1 to 6, characterized in that: When producing aromatic ketone, the reaction liquid is stored in a raw material tank (1). First, the heating device (6) is turned on to heat each section of the tubular reactor (5) to a set temperature. Then, the metering pump (3) is turned on to extract the reaction liquid in the raw material tank (1). The reaction liquid enters the tubular reactor (5) through the metering pump (3). The gas generated by the reaction enters the absorption tank (12) through the cooperation of the first condenser (8) and the second condenser (13), the first separator (9) and the second separator (14), and the exhaust pipe (19) to be absorbed by water. The entrained liquid material is returned to the tubular reactor (5) and the receiving tank (11) through the first separator (9) and the second separator (14), respectively. The material after the reaction is completed enters the receiving tank (11).

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