CN212595730U

CN212595730U - Grignard reaction fixed bed reactor

Info

Publication number: CN212595730U
Application number: CN202020922751.XU
Authority: CN
Inventors: 周留扣; 杨智深; 徐小海; 蔡继元
Original assignee: Jiangxi Chibang Pharmaceutical Co ltd
Current assignee: Jiangxi Chibang Pharmaceutical Co ltd
Priority date: 2020-05-27
Filing date: 2020-05-27
Publication date: 2021-02-26
Anticipated expiration: 2030-05-27

Abstract

The utility model discloses a Grignard reaction fixed bed reactor belongs to the fixed bed reactor field. In order to achieve the above purpose, the utility model adopts the following technical scheme: a Grignard reaction fixed bed reactor comprises a reactor body, wherein a fixed plate is connected to the inner wall of the bottom of the reactor body, a round hole is formed in the fixed plate, and a first filter screen is arranged in the round hole; the outer wall of the reactor body is also connected with a radiator and a circulating pump; a second pipeline is connected to the circulating pump, one end of the second pipeline, which is far away from the circulating pump, is connected with a filter tank, the outer wall of the filter tank is also connected with a fourth pipeline, and one end of the fourth pipeline, which is far away from the filter tank, penetrates through the reactor body and is connected to the bottom of the fixing plate; the fourth pipeline is connected with a third pipeline through a three-way pipe, and the third pipeline is connected with a circulating pump; the utility model discloses can circulate the reaction, make the reaction more abundant thoroughly, convenient operation has improved work efficiency.

Description

Grignard reaction fixed bed reactor

Technical Field

The utility model relates to a grignard reaction equipment technical field especially relates to a grignard reaction fixed bed reactor.

Background

Grignard reagent, originated in 1901 by the french chemist grignard. Organic halogen compound (alkyl halide, active aryl halide) and magnesium metal react in absolute anhydrous ether to form organic magnesium reagent.

The conventional preparation of the Grignard reagent is completed by adopting a batch mode. In a reaction bottle or a reaction kettle, firstly, metal magnesium, an initiator and a small amount of solvent are placed at the bottom of the reaction bottle or the reaction kettle, then, part of halide is dripped from the upper part of the reaction kettle or the reaction bottle, the residual halide is continuously dripped after initiation to form the magnesium halide, the metal magnesium is dissolved and converted into a Grignard reagent in the reaction process, the reaction is an exothermic reaction, heat is released by condensation and reflux, and after the reaction is finished, the excessive metal magnesium is removed by filtration.

In the existing Grignard reaction, after all the halogenated materials are added to form the Grignard reagent, the Grignard reagent can be discharged from the reaction kettle to continuously carry out the next batch reaction, and the relative work efficiency is low.

SUMMERY OF THE UTILITY MODEL

The utility model aims at solving the problems in the prior art and providing a Grignard reaction fixed bed reactor.

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

a Grignard reaction fixed bed reactor comprises a reactor body, wherein a fixed plate is connected to the inner wall of the bottom of the reactor body, a round hole is formed in the fixed plate, and a first filter screen is arranged in the round hole;

the outer wall of the reactor body is also connected with a radiator and a circulating pump, the radiator is connected with the circulating pump through a connecting pipe, and the radiator is communicated with the reactor body through a first pipeline;

a second pipeline is connected to the circulating pump, one end of the second pipeline, which is far away from the circulating pump, is connected with a filter tank, the outer wall of the filter tank is also connected with a fourth pipeline, and one end of the fourth pipeline, which is far away from the filter tank, penetrates through the reactor body and is connected to the bottom of the fixing plate;

and the fourth pipeline is connected with a third pipeline through a three-way pipe, and the third pipeline is connected with an air pump.

Preferably, the outer wall of the reactor body is fixedly connected with an annular plate, the outer wall of the annular plate is connected with a supporting plate, and the radiator and the circulating pump are respectively connected to the outer walls of the upper end and the lower end of the supporting plate.

Preferably, the inner wall of the filtering tank is also provided with a plurality of layers of second filter screens, the outer wall of the top of the filtering tank is also connected with an exhaust pipe, the outer wall of the top of the supporting plate is connected with a collecting tank, and the exhaust pipe is connected with the collecting tank.

Preferably, the bottom of the annular plate is connected with a supporting foot.

Preferably, the top outer wall of the reactor body is connected with a feeder, the top outer wall of the feeder is respectively connected with a first feeding pipe and a second feeding pipe, and the bottom of the reactor body is provided with a discharge pipe.

Preferably, the outer wall of the top of the reactor body is further connected with a condenser, and the condenser is connected with a condensing pipe.

Compared with the prior art, the utility model provides a grignard reaction fixed bed reactor possesses following beneficial effect:

1. the Grignard reaction fixed bed reactor firstly injects a solution mixed by tetrahydrofuran/toluene and a halide (such as chlorobenzene) into the bottom of a reactor body through an air pump, a third pipeline and a fourth pipeline, wherein the toluene/tetrahydrofuran is used as a solvent, the chlorobenzene is used as a reaction raw material, the three form a mixed solution, then the mixed solution moves upwards from round holes on a fixed plate along with the increase of the solution, the round holes are distributed in a circumference way and can be more dispersed, the reaction effect is enhanced, meanwhile, magnesium chips are added through a second feeding pipe on a feeder, and are enabled to move downwards in the reactor body so as to be matched with the solution for reaction, the first feeding pipe can discharge air in the reactor body, the Grignard damage of oxygen or water vapor is avoided, the reaction effect is enhanced, and materials after the reaction or rising to the first pipeline can be under the action of a circulating pump, get into first pipeline, then carry out the heat transfer through the radiator, then through the second pipeline with cross the filter tank, be equipped with the second filter screen in crossing the filter tank, then can filter it, then get into the below of fixed plate through the fourth pipeline, carry out the circulation operation, the reaction is more thorough, cross the filter tank and can collect the collection jar in through the blowing pipe with the result after filtering simultaneously, obtain grignard reagent, the condenser can carry out the condensation and release heat, the adjustment pressure.

The part that does not relate to in the device all is the same with prior art or can adopt prior art to realize, the utility model discloses can circulate the reaction, make the reaction more abundant thoroughly, convenient operation has improved work efficiency.

Drawings

Fig. 1 is a schematic structural diagram of a grignard reaction fixed bed reactor provided by the present invention;

FIG. 2 is a schematic structural view of a portion A of a fixed bed reactor in Grignard reaction in FIG. 1 according to the present invention;

fig. 3 is a schematic structural diagram of a portion B in fig. 1 of a grignard reaction fixed bed reactor according to the present invention.

In the figure: 1. a reactor body; 101. an annular plate; 102. supporting legs; 2. a fixing plate; 201. a circular hole; 202. a first filter screen; 3. a support plate; 4. a heat sink; 401. a first conduit; 5. a first circulating pump; 501. a second conduit; 6. a second circulating pump; 601. a third pipeline; 7. A filter tank; 701. a second filter screen; 702. a fourth conduit; 8. a collection tank; 9. a feeder; 901. a first feed tube; 902. a second feed tube; 10. a condenser.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.

Example (b):

referring to fig. 1-3, a grignard reaction fixed bed reactor comprises a reactor body 1, a fixed plate 2 is connected to the inner wall of the bottom of the reactor body 1, a circular hole 201 is formed in the fixed plate 2, and a first filter screen 202 is arranged in the circular hole 201;

the outer wall of the reactor body 1 is also connected with a radiator 4 and a first circulating pump 5, the radiator 4 is connected with the first circulating pump 5 through a connecting pipe, and the radiator 4 is communicated with the reactor body 1 through a first pipeline 401;

a second pipeline 501 is connected to the first circulating pump 5, one end, far away from the first circulating pump 5, of the second pipeline 501 is connected with a filter tank 7, the outer wall of the filter tank 7 is further connected with a fourth pipeline 702, and one end, far away from the filter tank 7, of the fourth pipeline 702 penetrates through the reactor body 1 and is connected to the bottom of the fixing plate 2;

the fourth pipeline 702 is connected with a third pipeline 601 through a three-way pipe, and the third pipeline 601 is connected with a second circulating pump 6.

The outer wall of the reactor body 1 is fixedly connected with an annular plate 101, the outer wall of the annular plate 101 is connected with a supporting plate 3, and a radiator 4 and a circulating pump I5 are respectively connected to the outer walls of the upper end and the lower end of the supporting plate 3.

The inner wall of the filtering tank 7 is also provided with a plurality of layers of second filtering nets 701, the outer wall of the top of the filtering tank 7 is also connected with an exhaust pipe, the outer wall of the top of the supporting plate 3 is connected with a collecting tank 8, and the exhaust pipe is connected with the collecting tank 8.

The bottom of the annular plate 101 is connected with a support foot 102.

The top outer wall of reactor body 1 is connected with charging means 9, and the top outer wall of charging means 9 is connected with first filling tube 901 and second filling tube 902 respectively, and the bottom of reactor body 1 is equipped with the discharge tube.

The outer wall of the top of the reactor body 1 is also connected with a condenser 10, and the condenser 10 is connected with a condensing pipe.

In the utility model, firstly, the solution mixed with toluene and chlorobenzene is injected into the bottom of the reactor body 1 through the second circulating pump 6, the third pipeline 601 and the fourth pipeline 702, wherein toluene/tetrahydrofuran is used as solvent, halogenated substances are used as raw materials, the mixed solution is formed, then the solution is increased along with the short time of the solution, then the solution moves upwards from the round hole 201 on the fixed plate 2, the round hole 201 is distributed in a circumference, the solution can be more dispersed, the reaction effect is enhanced, meanwhile, magnesium chips are added through the second feeding pipe 902 on the feeder 9, the solution moves downwards in the reactor body 1 by self weight, so as to be matched with the solution for reaction, the first feeding pipe 901 can discharge the air in the reactor body 1, the damage of oxygen or water vapor to Grignard is avoided, so as to enhance the reaction effect, the material after the reaction or ascending to the first pipeline 401 can be under the action of the first circulating pump 5, get into first pipeline 401, then carry out the heat transfer through radiator 4, then through second pipeline 501 and filter tank 7, be equipped with second filter screen 701 in the filter tank 7, then can filter it, then get into the below of fixed plate 2 through fourth pipeline 702, carry out the circulation operation, the reaction is more thorough, filter tank 7 simultaneously can be with the result after filtering in collecting tank 8 is collected through the connecting pipe, avoid its direct discharge polluted environment, and condenser 10 can carry out the condensation and release heat, the adjustment pressure.

The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.

Claims

1. A Grignard reaction fixed bed reactor comprises a reactor body (1), and is characterized in that the inner wall of the bottom of the reactor body (1) is connected with a fixed plate (2), a round hole (201) is arranged on the fixed plate (2), and a first filter screen (202) is arranged in the round hole (201);

the reactor is characterized in that the outer wall of the reactor body (1) is also connected with a radiator (4) and a first circulating pump (5), the radiator (4) is connected with the first circulating pump (5) through a connecting pipe, and the radiator (4) is communicated with the reactor body (1) through a first pipeline (401);

a second pipeline (501) is connected to the first circulating pump (5), one end, far away from the first circulating pump (5), of the second pipeline (501) is connected with a filtering tank (7), the outer wall of the filtering tank (7) is further connected with a fourth pipeline (702), and one end, far away from the filtering tank (7), of the fourth pipeline (702) penetrates through the reactor body (1) and is connected to the bottom of the fixing plate (2);

the fourth pipeline (702) is connected with a third pipeline (601) through a three-way pipe, and the third pipeline (601) is connected with a second circulating pump (6).

2. The grignard reaction fixed bed reactor according to claim 1, wherein the outer wall of the reactor body (1) is fixedly connected with an annular plate (101), the outer wall of the annular plate (101) is connected with a support plate (3), and the heat sink (4) and the first circulation pump (5) are respectively connected to the outer walls of the upper end and the lower end of the support plate (3).

3. The fixed bed reactor of claim 2, characterized in that the inner wall of the filtering tank (7) is further provided with a plurality of layers of second filter screens (701), the outer wall of the top of the filtering tank (7) is further connected with a discharging pipe, the outer wall of the top of the supporting plate (3) is connected with the collecting tank (8), and the discharging pipe is connected with the collecting tank (8).

4. A grignard fixed bed reactor according to claim 2, characterized in that the bottom of the annular plate (101) is connected with support legs (102).

5. The grignard reaction fixed bed reactor according to claim 1, wherein the top outer wall of the reactor body (1) is connected with a feeder (9), the top outer wall of the feeder (9) is respectively connected with a first feeding pipe (901) and a second feeding pipe (902), and the bottom of the reactor body (1) is provided with a discharge pipe.

6. The Grignard fixed bed reactor according to claim 5, characterized in that the top outer wall of the reactor body (1) is further connected with a condenser (10), and the condenser (10) is connected with a condensing tube.