CN215028800U - Liquid membrane nitration reaction device - Google Patents
Liquid membrane nitration reaction device Download PDFInfo
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- CN215028800U CN215028800U CN202120257271.0U CN202120257271U CN215028800U CN 215028800 U CN215028800 U CN 215028800U CN 202120257271 U CN202120257271 U CN 202120257271U CN 215028800 U CN215028800 U CN 215028800U
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Abstract
The utility model relates to a liquid membrane nitration reaction device, which comprises a reactor body, a rotary membrane scraping mechanism, a heating jacket and a middle condensation column; the rotary film scraping mechanism consists of a motor, a rotating shaft, a material throwing disc and a film scraping cylinder. The device of the utility model is suitable for the production of nitration products in laboratory-level production or industrial production; the method is convenient for observing the reaction phenomenon in the reaction device, optimizes the reaction by controlling the feeding ratio and the reaction temperature, and can recover the solvent while reacting; the device has the advantages of simple structure, convenient and quick material feeding, accurate control and easy equipment operation and cleaning.
Description
Technical Field
The utility model relates to a nitration technical field especially relates to a liquid membrane nitration device.
Background
The nitration reaction is a process of introducing a nitro group into an organic compound molecule, and the nitro group is a univalent group formed by nitric acid losing one hydroxyl group. The reaction mechanism of the nitration of aromatic compounds is as follows: the hydroxyl group of nitric acid is protonated, then one molecule of water is removed by the dehydrating agent to form a nitroxyl positive ion intermediate, and finally, electrophilic aromatic substitution reaction is carried out on the intermediate and a benzene ring, and one molecule of hydrogen ion is removed.
The nitration reaction apparatuses commonly used today are basically two types, one is a reaction kettle and the other is a microreactor.
The conventional reaction kettle is designed in a double-layer mode, reaction solvent is placed in the inner layer, a stirring device is arranged, and different cold and heat sources (refrigerating fluid, hot water or hot oil) can be introduced into the interlayer for circulating heating or cooling. The reaction can be carried out under normal pressure or negative pressure in the sealed enamel glass reaction kettle under the set constant temperature condition according to the use requirement, and the reflux and distillation of the reaction solution can be carried out, so the reaction kettle is ideal pilot plant test and production equipment for modern fine chemical engineering, biological pharmacy and new material synthesis.
However, the conventional reaction kettle also has some defects, such as potential safety hazards of flammability, explosiveness, toxicity, corrosion and the like during working, which can harm the personal safety and the property safety to different degrees and also influence the product quality. By adopting the traditional kettle type reactor, the heat released by the reaction can not be released in time, and the reaction temperature can not be accurately controlled. The reaction rate is often artificially severely limited, otherwise explosions may occur. According to statistics, on average, forty major safety accidents related to the reaction kettle are caused in China every year. It is therefore desirable to carry out such reactions using other more suitable reaction apparatus.
The micro-reactor can overcome the defects of a tank reactor, a plurality of academic reports compare the traditional reactor with the micro-reactor at present, and the micro-reactor is found to be more capable of strengthening the reaction process than the traditional reactor. Microreactors are also known as micro hydrogenation reactors, micro magnetic high pressure reactors. Has the advantages of high temperature resistance, corrosion resistance, strong production capacity and the like, and is widely applied to the industrial departments of medicine, beverage, chemical industry, pigment, resin, scientific research and the like.
However, the micro-reactor is very complex to operate for industrial applications: when the number of microreactors is greatly increased, the complexity of monitoring and controlling the microreaction is also greatly increased, and the cost is relatively high for practical production. And the micro-channel inside the micro-reactor has small size and complex structure, so that the channel of the reactor is easy to block and is difficult to clean. This has been a major challenge in microreactor applications.
Disclosure of Invention
The utility model provides a liquid membrane nitration reaction device, which is suitable for the production of nitration products in laboratory-level production or industrial production; the method is convenient for observing the reaction phenomenon in the reaction device, optimizes the reaction by controlling the feeding ratio and the reaction temperature, and can recover the solvent while reacting; the device has the advantages of simple structure, convenient and quick material feeding, accurate control and easy equipment operation and cleaning.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a liquid membrane nitration reaction device comprises a reactor body, a rotary membrane scraping mechanism, a heating jacket and a middle condensation column; the rotary film scraping mechanism consists of a motor, a rotating shaft, a material throwing disc and a film scraping cylinder; the top of the reactor body is provided with a through hole, the motor is fixedly arranged above the reactor body, the upper end of the rotating shaft is connected with the motor shaft, and the lower end of the rotating shaft extends into the reactor body from the through hole and is connected with the film scraping cylinder; a feed inlet is arranged at the upper part of the reactor body, a material throwing disc is arranged on a rotating shaft above the film scraping barrel in the reactor body, and the feed inlet is arranged at one side above the material throwing disc; a gap is reserved between the inner wall of the reactor body and the outer wall of the film scraping cylinder, and the reactor body is provided with a heating jacket at the outer side corresponding to the film scraping cylinder; the middle part of the reactor body is provided with a middle condensation column, the lower part of the reactor body is provided with a steam outlet and a heavy component outlet, and the bottom of the reactor body is provided with a light component outlet.
The feed inlet is 2, sets up one on the other, get rid of the charging tray and be 2 layers, the feed inlet sets up with getting rid of the charging tray one-to-one.
The inlet pipe is established to the feed inlet, and the inlet pipe inwards extends to 1/2 radius departments of getting rid of the charging tray.
And a plurality of inclined grooves are formed outside the film scraping cylinder.
The bottom of the heating jacket is provided with a hot oil inlet, and the top of the heating jacket is provided with a hot oil outlet.
The middle condensation column is of a sleeve structure consisting of an inner tube and an outer tube, the bottom end of the middle condensation column extends out of the reactor body, the bottom of the outer tube is provided with a cold water inlet, and the bottom of the inner tube is provided with a cold water outlet.
The steam outlet and the heavy component outlet are respectively arranged at two sides of the reactor body, the steam outlet is higher than the heavy component outlet and is obliquely arranged towards the outer upper part and the heavy component outlet towards the outer lower part.
The reactor body is provided with an inner extension pipe at the outer side of the lower part corresponding to the middle condensation column, and the lower end of the middle condensation column penetrates out of the lower part of the inner extension pipe; the light component outlet is arranged at one side of the bottom of the inner extension pipe and is obliquely arranged towards the outer lower part.
Compared with the prior art, the beneficial effects of the utility model are that:
1) by arranging more than 2 material throwing discs, multi-component raw material mixing can be realized, and the raw material proportion is conveniently controlled;
2) the reaction temperature can be accurately controlled at any time by adjusting the temperature of hot oil introduced into the heating jacket;
3) the middle part of the reactor body is provided with a middle condensation column which can condense and recover the volatile solvent in the reactor body;
4) the whole structure is simple, the manufacturing cost is low, the operation and the cleaning are convenient, and the energy consumption is saved; is beneficial to reducing the production cost of the product and has strong market competitiveness.
Drawings
FIG. 1 is a schematic structural diagram of a liquid membrane nitration apparatus of the present invention.
In the figure: 1. the device comprises a motor 2, a feed inlet 3, a material throwing disc 4, a film scraping barrel 5, a heating jacket 6, a heavy component outlet 7, a hot oil inlet 8, a hot oil outlet 9, a light component outlet 10, a cold water inlet 11, a cold water outlet 12 and a steam outlet
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings:
as shown in fig. 1, the liquid membrane nitration apparatus of the present invention comprises a reactor body, a rotary membrane scraping mechanism, a heating jacket 5 and a middle condensation column; the rotary film scraping mechanism consists of a motor 1, a rotating shaft, a material throwing plate 3 and a film scraping cylinder 4; the top of the reactor body is provided with a through hole, the motor 1 is fixedly arranged above the reactor body, the upper end of the rotating shaft is connected with a motor shaft, and the lower end of the rotating shaft extends into the reactor body from the through hole and is connected with the film scraping cylinder 4; a feed inlet 2 is arranged at the upper part of the reactor body, a material throwing disc 3 is arranged on a rotating shaft above the film scraping cylinder 4 in the reactor body, and the feed inlet 2 is arranged at one side above the material throwing disc 3; a gap is reserved between the inner wall of the reactor body and the outer wall of the film scraping cylinder 4, and the reactor body is provided with a heating jacket 5 at the outer side corresponding to the film scraping cylinder 4; the middle part of the reactor body is provided with a middle condensation column, the lower part of the reactor body is provided with a steam outlet 12 and a heavy component outlet 6, and the bottom of the reactor body is provided with a light component outlet 9.
The feed inlet 2 is 2, sets up one on the other, it is 2 layers to get rid of charging tray 3, feed inlet 2 sets up with getting rid of charging tray 3 one-to-one.
The feed inlet 2 is provided with a feed pipe which extends inwards to 1/2 radius of the material throwing disc 3.
And a plurality of inclined grooves are formed in the outer wall of the film scraping cylinder 4.
The bottom of the heating jacket 5 is provided with a hot oil inlet 7, and the top is provided with a hot oil outlet 8.
The middle condensation column is a sleeve structure consisting of an inner pipe and an outer pipe, the bottom end of the middle condensation column extends out of the reactor body, the bottom of the outer pipe is provided with a cold water inlet 10, and the bottom of the inner pipe is provided with a cold water outlet 11.
The steam outlet 12 and the heavy component outlet 6 are respectively arranged at two sides of the reactor body, the steam outlet 12 is higher than the heavy component outlet 6, the steam outlet 12 is obliquely arranged towards the outer upper part, and the heavy component outlet 6 is obliquely arranged towards the outer lower part.
The reactor body is provided with an inner extension pipe at the outer side of the lower part corresponding to the middle condensation column, and the lower end of the middle condensation column penetrates out of the lower part of the inner extension pipe; the light component outlet 9 is arranged at one side of the bottom of the inner extension pipe and is obliquely arranged outwards and downwards.
The utility model relates to a liquid membrane nitration reaction device, which comprises a reactor body, a rotary membrane scraping mechanism, a heating jacket 5 and a middle condensation column, wherein the reactor body, the heating jacket 5 and the middle condensation column are designed into a whole; the upper part of the reactor body is provided with 2 feed inlets 2, the middle part is provided with a heating jacket 5, and the lower part is provided with three discharge outlets, namely a heavy component outlet 6, a light component outlet 9 and a steam outlet 12.
2 the inlet pipe is established to 2 departments of individual feed inlet, and the inlet pipe inwards extends to the 1/2 radius departments of getting rid of charging tray 3, and the material adds gets rid of the charging tray 3 and goes up the back, along with getting rid of charging tray 3 horizontal rotation under the drive of motor 1, evenly spreads to the inner wall of reactor body under the centrifugal force effect, at this in-process, makes the material homogeneous mixing.
Establish in the reactor body and scrape a membrane section of thick bamboo 4, be equipped with a plurality of oblique recesses at the interval on the outer wall of a membrane section of thick bamboo 4, scrape a membrane section of thick bamboo 4 and rotate along with the pivot, the raw materials that flows down from the reactor body inner wall is spread into the liquid film form under the effect of a membrane section of thick bamboo 4, further mixes and reacts in oblique recess.
The reactor body is provided with a heating jacket 5 at the outer side corresponding to the film scraping cylinder 4, the heating jacket 5 is provided with a hot oil outlet 8 and a hot oil inlet 7, and the reactor body is heated by hot oil circulation to provide the temperature required by the reaction.
The intermediate condenser is provided with a cold water inlet 10 and a cold water outlet 11, and is used for condensing the solvent volatilized in the reaction process through cold water circulation, so that the solvent recovery is realized.
And the heavy component, the light component and the gas phase after the reaction are respectively discharged out of the reactor body from corresponding outlets.
The utility model relates to a use method of a liquid membrane nitration reaction device, which comprises the following steps:
1) dissolving raw materials (organic compounds such as phthalic anhydride and the like) into liquid through an organic solvent (such as acetic acid, acetic anhydride, dichloroethane and the like), adding the raw materials and a nitrating agent (such as concentrated nitric acid or mixed acid of the concentrated nitric acid and the concentrated sulfuric acid and the like) onto corresponding material throwing discs 3 from different feed inlets 2, and driving the material throwing discs 3 to rotate by a motor 1 through a rotating shaft so that the raw materials are diffused to the edges of the material throwing discs 3 and flow downwards along the inner wall of the reactor body;
2) the materials react under the heating action of the heating jacket 5, the film scraping cylinder 4 is driven by the motor 1 to rotate, the raw materials are uniformly mixed and fully react in the inclined groove, and the reacted heavy components flow downwards to the lower part of the reactor body and are discharged through a heavy component outlet 6;
3) in the reaction process, the solvent is volatilized continuously, is condensed under the action of the middle condensing column, flows downwards along the outer wall of the middle condensing column and is discharged through the light component outlet 9;
4) the gas phase produced during the reaction is discharged through the steam outlet 12.
The following examples are carried out on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the following examples. The methods used in the following examples are conventional methods unless otherwise specified.
[ example 1 ]
In the embodiment, a liquid membrane nitration reaction device is adopted to carry out a phthalic anhydride nitration reaction test; the upper part of the reactor body is provided with 2 feed inlets one above the other, and correspondingly, the rotating shaft is provided with 2 layers of material throwing discs; the specific test process is as follows:
1. and starting the motor to rotate the material throwing disc and the film scraping cylinder.
2. Hot oil heated to 70 ℃ is input into the heating jacket from a hot oil inlet, flows from bottom to top in the heating jacket and flows out from a hot oil outlet at the upper part to form circulation, so that the reaction temperature is kept constant. Meanwhile, cold water is injected into the middle condensation column to form circulation.
3. Dissolving 50% phthalic anhydride by mass, preparing dichloroethane solution with corresponding concentration, and feeding the dichloroethane solution onto the lower oil thrower from the lower feeding port at a speed of 8 ml/min; concentrated sulfuric acid and concentrated nitric acid are mixed according to the mass ratio of 1: 1.2 after mixing, the mixture is put into an oil thrower on the upper layer from an upper feeding port at a rate of 8 ml/min.
After 3 hours of reaction, 0.98kg of product was obtained, the product yield was 84.81%, and the recovered solvent was substantially free of impurities. All properties of the product meet the requirements, and the determination is qualified.
[ example 2 ]
In the embodiment, a liquid membrane nitration reaction device is adopted to carry out a phthalic anhydride nitration reaction test; the upper part of the reactor body is provided with 2 feed inlets one above the other, and correspondingly, the rotating shaft is provided with 2 layers of material throwing discs; the specific test process is as follows:
1. and starting the motor to rotate the material throwing disc and the film scraping cylinder.
2. Hot oil heated to 65 ℃ is input into the heating jacket from a hot oil inlet, flows from bottom to top in the heating jacket and flows out from a hot oil outlet at the upper part to form circulation, so that the reaction temperature is kept constant. Meanwhile, cold water is injected into the middle condensation column to form circulation.
3. Dissolving 50% phthalic anhydride by mass, preparing dichloroethane solution with corresponding concentration, and feeding the dichloroethane solution onto the lower oil thrower from the lower feeding port at a speed of 8 ml/min; concentrated sulfuric acid and concentrated nitric acid are mixed according to the mass ratio of 1: 1.1 after mixing, the mixture is fed into an oil thrower on the upper layer from an upper feeding port at a rate of 8 ml/min.
After 3 hours of reaction, 0.92kg of product was obtained, the product yield was 79.63%, and the recovered solvent was substantially free of impurities. All properties of the product meet the requirements, and the determination is qualified.
The above description is only the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the concept of the present invention within the technical scope disclosed in the present invention.
Claims (8)
1. A liquid membrane nitration reaction device is characterized by comprising a reactor body, a rotary membrane scraping mechanism, a heating jacket and a middle condensation column; the rotary film scraping mechanism consists of a motor, a rotating shaft, a material throwing disc and a film scraping cylinder; the top of the reactor body is provided with a through hole, the motor is fixedly arranged above the reactor body, the upper end of the rotating shaft is connected with the motor shaft, and the lower end of the rotating shaft extends into the reactor body from the through hole and is connected with the film scraping cylinder; a feed inlet is arranged at the upper part of the reactor body, a material throwing disc is arranged on a rotating shaft above the film scraping barrel in the reactor body, and the feed inlet is arranged at one side above the material throwing disc; a gap is reserved between the inner wall of the reactor body and the outer wall of the film scraping cylinder, and the reactor body is provided with a heating jacket at the outer side corresponding to the film scraping cylinder; the middle part of the reactor body is provided with a middle condensation column, the lower part of the reactor body is provided with a steam outlet and a heavy component outlet, and the bottom of the reactor body is provided with a light component outlet.
2. The liquid film nitration reaction device according to claim 1, wherein the number of the feed inlets is 2, the feed throwing plates are arranged one above the other, the number of the feed throwing plates is 2, and the feed inlets and the feed throwing plates are arranged in one-to-one correspondence.
3. The liquid film nitration reaction device as claimed in claim 1 or 2, wherein the feed inlet is provided with a feed pipe, and the feed pipe extends inwards to 1/2 radius of the material throwing disc.
4. The liquid membrane nitration reaction device as claimed in claim 1, wherein the outer wall of the membrane scraping cylinder is provided with a plurality of inclined grooves.
5. The liquid membrane nitration reaction device according to claim 1, wherein the heating jacket is provided with a hot oil inlet at the bottom and a hot oil outlet at the top.
6. The liquid membrane nitration reaction device according to claim 1, wherein the intermediate condensation column is a sleeve structure composed of an inner tube and an outer tube, the bottom end of the intermediate condensation column extends out of the reactor body, the bottom of the outer tube is provided with a cold water inlet, and the bottom of the inner tube is provided with a cold water outlet.
7. The liquid membrane nitration reaction device according to claim 1, wherein the steam outlet and the heavy component outlet are respectively arranged at two sides of the reactor body, the steam outlet is higher than the heavy component outlet, the steam outlet is obliquely arranged outwards and upwards, and the heavy component outlet is obliquely arranged outwards and downwards.
8. The liquid membrane nitration reaction device according to claim 1, wherein the reactor body is provided with an inner extension pipe at the outer side of the lower part corresponding to the middle condensation column, and the lower end of the middle condensation column penetrates out from the lower part of the inner extension pipe; the light component outlet is arranged at one side of the bottom of the inner extension pipe and is obliquely arranged towards the outer lower part.
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| CN202120257271.0U CN215028800U (en) | 2021-01-29 | 2021-01-29 | Liquid membrane nitration reaction device |
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| CN202120257271.0U CN215028800U (en) | 2021-01-29 | 2021-01-29 | Liquid membrane nitration reaction device |
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