CN215464394U

CN215464394U - Production device of chalcone compound catalyzed by diethyl methylphosphonite

Info

Publication number: CN215464394U
Application number: CN202121533477.8U
Authority: CN
Inventors: 吕从高; 刘宁; 李君柱; 戴先周; 孙陈; 周绪双
Original assignee: Honghu Yitai Technology Co ltd
Current assignee: Honghu Yitai Technology Co ltd
Priority date: 2021-07-06
Filing date: 2021-07-06
Publication date: 2022-01-11
Anticipated expiration: 2031-07-06

Abstract

The utility model discloses a production device of chalcone compounds catalyzed by diethyl methylphosphonite. The device comprises an enamel reaction kettle, a lower discharging centrifugal machine, drying equipment, a storage tank and a distillation kettle; the discharge hole of the enamel reaction kettle is communicated with the feed inlet of a lower discharge centrifugal machine, the discharge hole of the lower discharge centrifugal machine is communicated with the feed inlet of drying equipment, and the discharge hole of the drying equipment is communicated with a storage tank; the enamel reaction kettle is provided with a plurality of material charging ports and air inlets, and the air inlets are communicated with the nitrogen source; the liquid outlet of the lower discharging centrifuge is communicated with the feed inlet of the distillation kettle. The device is beneficial to the rearrangement of the diethyl methylphosphonite to generate ethoxy anions, improves the catalytic activity, and has the advantages of faster reaction rate, improved conversion rate, reduced side reactions, high product yield and stable product quality. Meanwhile, the filtrate is recycled and can be circularly applied to production, so that the production cost is reduced. Moreover, the reaction process is easy to control, the operation is simple and convenient, and the method is suitable for large-scale production.

Description

Production device of chalcone compound catalyzed by diethyl methylphosphonite

Technical Field

The utility model relates to the technical field of production of chalcone compounds, in particular to a production device of chalcone compounds catalyzed by diethyl methylphosphonite.

Background

The formation of carbon-carbon bonds is the most important and fundamental reaction in organic synthesis. The michael addition is recognized as the most efficient route for forming carbon-carbon bonds and is widely used in organic synthesis. The michael addition reaction is then typically carried out in the presence of a strong base, which causes some reactive functional groups to undergo side reactions, such as polymerization, etc. Under the catalysis of weak base, the Michael addition of unsaturated carbonyl compounds is improved to a certain extent, but the reaction time is long, and the yield can only reach a moderate level. In order to overcome the above disadvantages of the Michael addition reaction, there have been proposed improvements using a phase transfer catalyst, a transition metal compound, a Lewis acid, and the like, and the catalysts are expensive, large in amount, long in reaction time, complicated in operation, and low in yield. There is still a need for a high efficiency catalyst to overcome the above problems.

The applicant researches and discovers that diethyl methylphosphonite as a catalyst is remarkable in Michael addition reaction of unsaturated carbonyl compounds, diethyl methylphosphonite is weak in alkalinity, and can generate ethoxy anions through self rearrangement in the reaction process, so that active hydrogen of malononitrile is captured to carry out Michael addition on corresponding substrates.

Therefore, the development of a production device capable of preparing chalcone compounds by using diethyl methylphosphonite as a catalyst on a large scale has very important practical significance for improving the application range of diethyl methylphosphonite and reducing the application cost.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide a device for producing chalcone compounds catalyzed by diethyl methylphosphonite, aiming at the defects of the prior art.

In order to achieve the purpose, the utility model adopts the following technical scheme:

the utility model relates to a production device of chalcone compounds catalyzed by diethyl methylphosphonite, which comprises an enamel reaction kettle, a lower discharge centrifuge, drying equipment, a storage tank and a distillation kettle;

the discharge hole of the enamel reaction kettle is communicated with the feed inlet of the lower discharge centrifugal machine, the discharge hole of the lower discharge centrifugal machine is communicated with the feed inlet of the drying equipment, and the discharge hole of the drying equipment is communicated with the storage tank; the enamel reaction kettle is provided with a plurality of material adding ports and a gas inlet, and the gas inlet is communicated with a nitrogen source;

and the liquid outlet of the lower discharging centrifugal machine is communicated with the feed inlet of the distillation kettle.

Further, enamel reactor's discharge gate pass through first pipeline with bottom discharge centrifuge's feed inlet intercommunication, bottom discharge centrifuge's discharge opening pass through material transfer pipeline with drying equipment's feed inlet intercommunication, bottom discharge centrifuge's leakage fluid dram pass through the second pipeline with stills's feed inlet intercommunication, all be provided with first chemical industry pump and first valve on first pipeline, material transfer pipeline and the second pipeline.

Further, the enamel reaction kettle comprises a kettle body, a jacket, a cover body and a stirring assembly, wherein the kettle body and the cover body are detachably connected, and the jacket is sleeved on the outer side of the kettle body; the stirring assembly comprises a stirring paddle and a stirring motor, the stirring paddle is arranged in the kettle body, and the top end of the stirring paddle penetrates through the center of the cover body and is detachably connected with the stirring motor; a discharge hole of the enamel reaction kettle is formed in the center of the bottom of the kettle body; the cover body is provided with a plurality of feeding ports and air inlets.

Furthermore, a water inlet is arranged on the side surface above the jacket, and a water outlet is arranged at the bottom of the jacket.

Further, the feeding ports are at least provided with 4 feeding ports.

Furthermore, at least two of the feeding ports are provided with solid feeding devices.

Furthermore, at least two of the feeding ports are communicated with the metering tank through a third pipeline, and a metering pump and a flow control valve are arranged on the third pipeline.

Furthermore, the production device also comprises a nitrogen guide pipe, wherein the nitrogen guide pipe comprises a guide pipe and a nozzle, one end of the guide pipe is inserted into the kettle body from the air inlet, and the nozzle is detachably arranged at one end of the guide pipe.

Furthermore, a condenser can be detachably arranged at a steam outlet of the distillation kettle, and an outlet of the condenser is communicated with the acetonitrile temporary storage tank.

Further, the drying apparatus comprises a rake dryer.

The technical scheme provided by the utility model has the beneficial effects that:

(1) according to the production device of the chalcone compound catalyzed by the diethyl methylphosphonite, provided by the utility model, under the action of the diethyl methylphosphonite catalyst, the Michael addition reaction of an unsaturated carbonyl compound is carried out in the enamel reaction kettle, nitrogen is introduced into the enamel reaction kettle before the reaction, the normal proceeding of the reaction is protected, the rearrangement of the diethyl methylphosphonite to generate ethoxy negative ions is facilitated, the catalytic activity is improved, the reaction rate is faster, the conversion rate is improved, the side reactions are reduced, the product yield is high, and the product quality is stable.

(2) Meanwhile, filtrate is recovered through a distillation still and can be circularly applied to production, so that the production cost is reduced.

(3) In addition, the production device of the chalcone compound catalyzed by diethyl methylphosphonite provided by the utility model is suitable for controlling the reaction process, is simple and convenient to operate, and is suitable for large-scale production.

Drawings

FIG. 1 is a schematic structural diagram of a chalcone compound catalyzed by diethyl methylphosphonite.

1. An enamel reaction kettle; 11. a kettle body; 111. a discharge hole of the enamel reaction kettle; 1111. a first pipeline; 12. a jacket; 121. a water inlet; 122. a water outlet; 13. a cover body; 131. a feeding port; 132. an air inlet; 133. a nitrogen gas conduit; 1331. an introducing pipe; 1332. a nozzle; 14. a stirring assembly; 141. a stirring paddle; 142. a stirring motor; 15. a metering tank; 151. a third pipeline; 1511. a metering pump; 1512. a flow control valve; 2. a lower discharge centrifuge; 21. a feed inlet of a lower discharge centrifuge; 22. a discharge opening of the lower discharge centrifuge; 221. a material transfer conduit; 23. a liquid outlet of the lower discharging centrifuge; 231. a second pipeline; 3. a drying device; 31. a feed inlet of a drying apparatus; 32. a discharge port of the drying device; 4. a storage tank; 5. a distillation kettle; 51. a feed inlet of the distillation still; 52. a steam outlet; 521. a condenser; 6. and (5) temporarily storing acetonitrile.

Detailed Description

The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.

As shown in figure 1, the production device of chalcone compounds catalyzed by diethyl methylphosphonite provided by the utility model comprises an enamel reaction kettle 1, a lower discharge centrifuge 2, a drying device 3, a storage tank 4 and a distillation kettle 5; the discharge port 111 of the enamel reaction kettle 1 is communicated with the feed port 21 of the lower discharge centrifuge 2, the discharge port 22 of the lower discharge centrifuge 2 is communicated with the feed port 31 of the drying equipment 3, and the discharge port 32 of the drying equipment 3 is communicated with the storage tank 4; the enamel reaction kettle 1 is provided with a plurality of material adding ports 131 and air inlets 132, and the air inlets 132 are communicated with a nitrogen source; the liquid outlet 23 of the lower discharging centrifuge is communicated with the feed inlet 51 of the distillation still 5. Sequentially and respectively adding acetonitrile, 1- (4-methoxyphenyl) -3- (4-chlorophenyl) -2-propylene-1-one, 1, 3-malononitrile and diethyl methylphosphonite into a plurality of material adding ports 131 of an enamel reaction kettle 1, introducing nitrogen into the enamel reaction kettle 1 through an air inlet 132, carrying out Michael addition reaction in the enamel reaction kettle 1 to separate out a large amount of solid, carrying out centrifugal filtration by a lower discharging centrifugal machine 2, and drying a filter cake by a drying device 3 to obtain a chalcone product with the purity of not less than 98%; the filtrate is recycled by a distillation still 5, and the obtained acetonitrile is reused in the production. The production device of the chalcone compound catalyzed by diethyl methylphosphonite provided by the utility model has the advantages of high production efficiency, low energy consumption and stable product quality. Under the action of a diethyl methylphosphonite catalyst, the Michael addition reaction of an unsaturated carbonyl compound is carried out in an enamel reaction kettle, nitrogen is introduced into the enamel reaction kettle before the reaction, the protection reaction is carried out normally, the rearrangement of diethyl methylphosphonite to generate ethoxy anions is facilitated, the catalytic activity is improved, the reaction rate is faster, the conversion rate is improved, the side reactions are reduced, the product yield is high, and the product quality is stable. Meanwhile, filtrate is recovered through a distillation still and can be circularly applied to production, so that the production cost is reduced. Moreover, the reaction process is easy to control, the operation is simple and convenient, and the production device is suitable for large-scale production.

Discharge gate 111 of enamel reactor communicates with feed inlet 21 of lower discharging centrifuge through first pipeline 1111, lower discharging centrifuge's discharge opening 22 through material transfer pipe 221 with drying equipment's feed inlet 31 intercommunication, lower discharging centrifuge's leakage fluid dram 23 communicates with retort's feed inlet 51 through second pipeline 231, all is provided with first chemical pump and first valve on first pipeline 1111, material transfer pipe 221 and the second pipeline 231. The material is transferred through the design pipeline, so that the operation of workers is facilitated, the device maintenance is facilitated for the workers, and the orderly production is ensured.

In order to realize the efficient catalysis and the selective Michael addition reaction by using the diethyl methylphosphonite as a catalyst, the enamel reaction kettle 1 can also comprise a kettle body 11, a jacket 12, a cover body 13 and a stirring assembly 14, wherein the kettle body 11 and the cover body 13 are detachably connected, and the jacket 12 is sleeved on the outer side of the kettle body 11; the stirring assembly 14 comprises a stirring paddle 141 and a stirring motor 142, the stirring paddle 141 is arranged in the kettle body 11, and the top end of the stirring paddle 141 penetrates through the center of the cover body 13 and is detachably connected with the stirring motor 142; a discharge hole 111 of the enamel reaction kettle is arranged at the center of the bottom of the kettle body 11; the cover 13 is provided with a plurality of charging ports 131 and air inlets 132.

In order to effectively adjust the temperature required for the reaction, the upper side of the jacket 12 is provided with a water inlet 121, and the bottom of the jacket 12 is provided with a water outlet 122.

According to the designed Michael addition reaction process route, at least 4 feeding ports 131 of the enamel reaction kettle are arranged. In order to reduce cross contamination between materials and facilitate the control of reaction process by the staff, two of the feeding ports 131 may be provided with a solid material feeder 1311, and for precise feeding and yield improvement, two of the feeding ports 131 may be communicated with the metering tank 15 through a third pipeline 151, and the third pipeline 151 may be further provided with a metering pump 1511 and a flow control valve 1512.

In order to ensure the catalytic efficiency and improve the product yield, the production apparatus may further include a nitrogen guide pipe 133, and the nitrogen guide pipe may have various structures, which are not limited herein, in this embodiment, in order to prevent the nitrogen guide pipe from being clogged and facilitate the cleaning and maintenance of workers, the nitrogen guide pipe 133 may include an inlet pipe 1331 and a nozzle 1332, one end of the inlet pipe 1331 is inserted into the kettle 11 from the gas inlet 132, and the nozzle 1332 is detachably disposed at one end of the inlet pipe 1331.

The steam outlet 52 of the distillation kettle 5 is detachably provided with a condenser 521, and the outlet of the condenser 521 is communicated with the acetonitrile temporary storage tank 6. The recovery of acetonitrile saves the production cost and reduces the environmental pollution.

The drying apparatus 3 may be a rake dryer in order to control the moisture in the process, improve the quality of the product and better achieve economic efficiency.

The following will explain in detail the apparatus for producing chalcone compounds catalyzed by diethyl methylphosphonite according to the present invention with reference to the examples.

Pumping 1.5 tons of acetonitrile into an enamel reaction kettle from a first metering tank 15, starting a stirring component 14, introducing nitrogen into a kettle body 11 through a nitrogen guide pipe 133 for protection, installing solid feeders 1311 at a first feeding port 131 and a second feeding port 131 of the enamel kettle, adding 1.36 tons of 1- (4-methoxyphenyl) -3- (4-chlorophenyl) -2-propylene-1 ketone into the enamel reaction kettle 1 through the solid feeders of the first feeding port 131, adding 330kg of 1, 3-malononitrile into the enamel reaction kettle 1 from the solid feeders of the first feeding port 131, fully stirring and dissolving, starting circulating cooling water of a jacket 12, controlling the temperature range in the enamel reaction kettle 1 to be 10-15 ℃, and slowly pumping 34kg of diethyl methylphosphonite from the second metering tank 15 through a metering pump 1511, the pumping speed is maintained to be not more than 30 ℃ in the enamel reaction kettle 1 through the flow control valve 1512, and after the pumping is finished, the stirring is kept at about 30 ℃ for 2 hours, so that a large amount of solid products are separated out in the enamel reaction kettle 1. Discharging the materials from the enamel reaction kettle 1 to a lower discharging centrifuge 2 for centrifugal filtration, washing a filter cake with acetonitrile, then placing the filter cake into a rake dryer 3, drying the filter cake for 2 hours at the temperature of 45 ℃ at the pressure of 2.67KPa to obtain chalcone products, wherein the melting point is 117-118 ℃, and storing the chalcone products in a storage tank 4. The filtrate and the washing liquid are combined and then transferred into a distillation kettle 5, and acetonitrile is distilled out at 2.67KPa and 45 ℃ to an acetonitrile temporary storage tank 6 for the next batch of reaction.

The above is not relevant and is applicable to the prior art.

While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the utility model, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the utility model as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.

Claims

1. A production device of chalcone compounds catalyzed by diethyl methylphosphonite is characterized in that: comprises an enamel reaction kettle (1), a lower discharge centrifuge (2), drying equipment (3), a storage tank (4) and a distillation kettle (5);

the discharge hole (111) of the enamel reaction kettle is communicated with the feed hole (21) of the lower discharge centrifugal machine, the discharge hole (22) of the lower discharge centrifugal machine is communicated with the feed hole (31) of the drying equipment, and the discharge hole (32) of the drying equipment is communicated with the storage tank (4); the enamel reaction kettle (1) is provided with a plurality of material adding ports (131) and a gas inlet (132), and the gas inlet (132) is communicated with a nitrogen source;

and a liquid outlet (23) of the lower discharging centrifugal machine is communicated with a feed inlet (51) of the distillation kettle.

2. The apparatus for producing chalcone compounds according to claim 1, wherein: enamel reactor's discharge gate (111) through first pipeline (1111) with discharge centrifuge's feed inlet (21) intercommunication down, discharge centrifuge's discharge opening (22) down through material conveying pipeline (221) with drying equipment's feed inlet (31) intercommunication, discharge centrifuge's leakage fluid dram (23) down through second pipeline (231) with stills's feed inlet (51) intercommunication, all be provided with first chemical industry pump and first valve on first pipeline (1111), material conveying pipeline (221) and second pipeline (231).

3. The apparatus for producing chalcone compounds according to claim 1, wherein: the enamel reaction kettle (1) comprises a kettle body (11), a jacket (12), a cover body (13) and a stirring assembly (14), wherein the kettle body (11) and the cover body (13) are detachably connected, and the jacket (12) is sleeved on the outer side of the kettle body (11); the stirring assembly (14) comprises a stirring paddle (141) and a stirring motor (142), the stirring paddle (141) is arranged in the kettle body (11), and the top end of the stirring paddle passes through the center of the cover body (13) and is detachably connected with the stirring motor (142); a discharge hole (111) of the enamel reaction kettle is formed in the center of the bottom of the kettle body (11); the cover body (13) is provided with a plurality of feeding ports (131) and air inlets (132).

4. The apparatus for producing chalcone compounds according to claim 3, wherein: a water inlet (121) is arranged on the side surface above the jacket (12), and a water outlet (122) is arranged at the bottom of the jacket (12).

5. The apparatus for producing chalcone compounds according to claim 3, wherein: the feeding ports (131) are at least provided with 4.

6. The apparatus for producing chalcone compounds according to claim 4, wherein: at least two of the feeding ports (131) are provided with a solid feeder (1311).

7. The apparatus for producing chalcone compounds according to claim 4, wherein: at least two of the feeding ports (131) are communicated with the metering tank (15) through a third pipeline (151), and a metering pump (1511) and a flow control valve (1512) are arranged on the third pipeline (151).

8. The apparatus for producing chalcone compounds according to claim 3, wherein: the production device also comprises a nitrogen guide pipe (133), wherein the nitrogen guide pipe (133) comprises an inlet pipe (1331) and a nozzle (1332), one end of the inlet pipe (1331) is inserted into the kettle body (11) from the air inlet (132), and the nozzle (1332) is detachably arranged at one end of the inlet pipe (1331).

9. The apparatus for producing chalcone compounds according to claim 1, wherein: a condenser (521) is detachably arranged at a steam outlet (52) of the distillation kettle (5), and an outlet of the condenser (521) is communicated with the acetonitrile temporary storage tank (6).

10. The apparatus for producing chalcone compounds according to claim 1, wherein: the drying apparatus (3) comprises a rake dryer.