CN214765371U

CN214765371U - System for rapidly synthesizing propiophenone from medical intermediate

Info

Publication number: CN214765371U
Application number: CN202120775728.7U
Authority: CN
Inventors: 郭继波; 周广鹏; 郭伟; 赵明波
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-04-16
Filing date: 2021-04-16
Publication date: 2021-11-19
Anticipated expiration: 2031-04-16

Abstract

The utility model discloses a system for quickly synthesizing propiophenone from a medical intermediate, which utilizes a reaction kettle with an internal baffle plate to quickly synthesize an epoxy resin curing agent, thereby achieving the production purposes of low consumption, high efficiency and cleanness; the technical scheme is as follows: the feeding port of the synthesis reaction kettle is connected with the outlet of the dripping tank, the inlet of the dripping tank is communicated with the aniline storage tank through a feeding pump, the discharging port of the synthesis reaction kettle is communicated with the feeding port of the hydrolysis reaction kettle, the feeding end of a first condenser is communicated with the upper volatilization port of the synthesis reaction kettle, the condensing end of the first condenser is connected to a recovery tank, the vacuumizing end of a synthesis vacuum system is respectively connected to the recovery tank, the synthesis reaction kettle and the hydrolysis reaction kettle, the feeding end of a reduced pressure distillation kettle is communicated with the discharging end of the hydrolysis reaction kettle, the discharging end of the reduced pressure distillation kettle is communicated with the feeding end of a second condenser, the condensing end of the second condenser is connected to a finished product tank, and the vacuumizing end of the vacuum system is connected to the finished product tank; the utility model discloses wide application in fine chemistry industry field.

Description

System for rapidly synthesizing propiophenone from medical intermediate

Technical Field

The utility model relates to a pharmaceutical intermediate synthesizes propiophenone system fast belongs to fine chemistry industry technical field.

Background

Propiophenone belongs to an aromatic ketone product, can be used as a general reagent, is an industrial intermediate for pharmacy, spice, essence and organic fine chemical synthesis, is an important chemical raw material, and can be used as a medical intermediate for synthesizing methytoin, cholestyrol, tamoxifen and the like as medicines.

SUMMERY OF THE UTILITY MODEL

The utility model overcomes the defects in the prior art, provides a medicine intermediate rapid synthesis propiophenone system, which utilizes a reaction kettle with an internal baffle plate to rapidly synthesize and react the medicine intermediate propiophenone, and achieves the production purposes of low consumption, high efficiency and cleanness.

In order to solve the technical problem, the utility model discloses a technical scheme be: a medicine intermediate rapid synthesis propiophenone system comprises a synthesis reaction kettle, a first condenser, a recovery tank, a dropping tank, a synthesis vacuum system, a hydrolysis reaction kettle, a reduced pressure distillation kettle, a second condenser, a finished product tank, a vacuum system and a feeding pump, wherein a feeding port of the synthesis reaction kettle is connected with an outlet of the dropping tank, an inlet of the dropping tank is communicated with a benzene storage tank through the feeding pump, a discharging port of the synthesis reaction kettle is communicated with a feeding port of the hydrolysis reaction kettle, a feeding end of the first condenser is communicated with a distillation port at the upper part of the synthesis reaction kettle, a condensing end of the first condenser is connected onto the recovery tank, a vacuumizing end of the synthesis vacuum system is respectively connected onto the recovery tank, the synthesis reaction kettle and the hydrolysis reaction kettle, a feeding end of the reduced pressure distillation kettle is communicated with a discharging end of the hydrolysis reaction kettle, a discharging end of the reduced pressure distillation kettle is communicated with a feeding end of the second condenser, and the condensation end of the second condenser is connected to the finished product tank, and the vacuumizing end of the vacuum system is connected to the finished product tank.

And the cooling layers of the first condenser and the second condenser are connected to a water circulation pipeline.

And pipelines in the walls of the synthesis reaction kettle and the hydrolysis reaction kettle are connected to a pipeline of the ice machine.

The water circulation pipeline is connected to the water circulation system.

The ice maker pipeline is connected to the ice maker system.

And the heating pipeline of the synthesis reaction kettle is communicated with the steam pipeline.

The steam pipeline is communicated with a steam heating system.

The structure of the synthesis reaction kettle is as follows: the device comprises a synthesis reaction kettle body, baffle plates, cooling pipes and stirring blades, wherein the baffle plates are vertically and uniformly distributed in the synthesis reaction kettle body, the cooling pipes are vertically distributed in the synthesis reaction kettle body in a plurality of annular arrangements, and the stirring blades are arranged on the upper part and the lower part in the synthesis reaction kettle body.

Compared with the prior art, the utility model beneficial effect who has is: the utility model discloses 6 pieces of H8 of equipartition in synthetic reation kettle 100 (1200) (304) boards impel benzene, propionyl chloride, aluminium trichloride to pass through acylation reaction and synthesize propiophenone fast, the utility model discloses rapid synthesis medicine intermediate propiophenone, propiophenone belong to important industrial chemicals for pharmacy, spices, essence and organic fine chemistry industry synthesis industrial intermediate belong to the general intermediate propiophenone of aromatic ketone class product.

Drawings

The present invention will be further described with reference to the accompanying drawings.

Fig. 1 is a schematic structural diagram of the present invention.

Fig. 2 is a schematic structural diagram of the middle synthesis reaction kettle of the utility model.

In the figure: 1 is a synthesis reaction kettle, 101 is a synthesis reaction kettle body, 102 is a baffle plate, 103 is a cooling pipe, 104 is a stirring blade, 2 is a first condenser, 3 is a recovery tank, 4 is a dropping tank, 5 is a synthesis vacuum system, 6 is a hydrolysis reaction kettle, 7 is a reduced pressure distillation kettle, 8 is a second condenser, 9 is a finished product tank, 10 is a vacuum system, 11 is a water circulation system, 12 is a steam heating system, 13 is an ice machine system, 14 is an ice machine pipeline, 15 is a feeding pump, 16 is a water circulation pipeline, 17 is a steam pipeline, and 18 is a benzene storage tank.

Detailed Description

As shown in figures 1 and 2, the utility model relates to a system for rapidly synthesizing propiophenone from a medical intermediate, which comprises a synthesis reaction kettle 1, a first condenser 2, a recovery tank 3, a dropwise adding tank 4, a synthesis vacuum system 5, a hydrolysis reaction kettle 6, a reduced pressure distillation kettle 7, a second condenser 8, a finished product tank 9, a vacuum system 10 and a feeding pump 15, wherein a feeding port of the synthesis reaction kettle 1 is connected with an outlet of the dropwise adding tank 4, an inlet of the dropwise adding tank 4 is communicated with a benzene storage tank 18 through the feeding pump 15, a discharging port of the synthesis reaction kettle 1 is communicated with a feeding port of the hydrolysis reaction kettle 6, a feeding port of the first condenser 2 is communicated with an upper volatilization port of the synthesis reaction kettle 1, a condensing end of the first condenser 2 is connected with the recovery tank 3, a vacuumizing end of the synthesis vacuum system 5 is respectively connected with the recovery tank 3, the synthesis reaction kettle 1 and the hydrolysis reaction kettle 6, the feed end of reduced pressure stills 7 and hydrolysis reaction cauldron 6's discharge end intercommunication, the discharge end of reduced pressure stills 7 and the feed end intercommunication of second condenser 8, the condensation end of second condenser 8 is connected on finished product jar 9, vacuum system 10's evacuation end is connected on finished product jar 9.

The cooling layers of the first condenser 2 and the second condenser 8 are both connected to a water circulation pipeline 16.

The pipelines in the walls of the synthesis reaction kettle 1 and the hydrolysis reaction kettle 6 are connected to an ice machine pipeline 14.

The water circulation line 16 is connected to the water circulation system 11.

The ice machine piping 14 is connected to the ice machine system 13.

The heating pipeline of the synthesis reaction kettle 1 is communicated with a steam pipeline 17.

The steam line 17 communicates with the steam heating system 12.

The structure of the synthesis reaction kettle 1 is as follows: the reaction kettle comprises a synthesis reaction kettle body 101, baffle plates 102, cooling pipes 103 and stirring blades 104, wherein the baffle plates 102 are vertically and uniformly distributed in the synthesis reaction kettle body 101, the cooling pipes 103 which are annularly arranged are vertically distributed in the synthesis reaction kettle body 101, and the stirring blades 104 are arranged on the upper part and the lower part in the synthesis reaction kettle body 101.

The utility model discloses a working process: 400kg of benzene and 1000kg of aluminum trichloride are put into a synthesis reaction kettle with a built-in baffle plate, the stirring speed is started to be controlled at 63 r/min, the rest 600kg of benzene and 330kg of propionyl chloride are pumped into an upper tank under the action of a synthesis vacuum system, the temperature of an ice machine system is controlled at 10 ℃, the synthesis reaction kettle is communicated through an ice machine pipeline, mixed reaction liquid (benzene and propionyl chloride) is dripped, the dripping time is controlled at 90min, and the weight ratio of propiophenone is produced (benzene 1: propionyl chloride 0.33: aluminum trichloride 0.55). After the dripping is finished, the temperature is raised to 75 ℃, reflux acylation reaction is carried out for 2 hours, benzene is evaporated out, the temperature of propiophenone in the synthesis reaction kettle is reduced to 20 ℃, a bottom valve is opened, the propiophenone enters the hydrolysis reaction kettle under the action of synthesis vacuum, 800kg of water is added into the hydrolysis reaction kettle, the temperature of the water is reduced in an ice machine system through an ice machine pipeline, the opening speed and the flow of the valve are strictly controlled when the ice water in the hydrolysis reaction kettle is controlled to be 0 ℃, the hydrolysis temperature of the hydrolysis reaction kettle is controlled not to exceed 20 ℃, the rest of layered water after the hydrolysis is finished is discharged, a catalyst is filtered out through a plate-frame filter, the crude propiophenone is neutralized through water washing, the crude propiophenone enters a reduced pressure distillation reaction kettle to start distillation under the action of a vacuum system, the temperature of heat conducting oil in the reduced pressure distillation kettle is controlled to be 180-200 ℃, the vacuum degree is controlled to be 0.97-0.98, the temperature of circulating water in a condenser is controlled to be 27-30 ℃, and the reduced pressure distillation temperature fraction is 112-120 ℃ propiophenone.

The utility model discloses 6 pieces of H8 of equipartition in reation kettle 100 (304) board, impel (benzene + aluminium trichloride), propionyl chloride, hydrolyze through the acylation and make medical intermediate propiophenone, the utility model discloses medical intermediate rapid synthesis propiophenone is used for propiophenone to belong to important industrial chemicals for pharmacy, spices, essence and the synthetic industry intermediate of organic meticulous chemical industry belong to the general intermediate propiophenone of aromatic ketone class product.

The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.

Claims

1. The system for rapidly synthesizing the propiophenone from the medical intermediate is characterized by comprising a synthesis reaction kettle (1), a first condenser (2), a recovery tank (3), a dropwise adding tank (4), a synthesis vacuum system (5), a hydrolysis reaction kettle (6), a reduced pressure distillation kettle (7), a second condenser (8), a finished product tank (9), a vacuum system (10) and a feeding pump (15), wherein a feeding port of the synthesis reaction kettle (1) is connected with an outlet of the dropwise adding tank (4), an inlet of the dropwise adding tank (4) is communicated with a benzene storage tank (18) through the feeding pump (15), a discharging port of the synthesis reaction kettle (1) is communicated with a feeding port of the hydrolysis reaction kettle (6), a feeding end of the first condenser (2) is communicated with an upper evaporation port of the synthesis reaction kettle (1), a condensing end of the first condenser (2) is connected to the recovery tank (3), the evacuation end of synthetic vacuum system (5) is connected respectively on recovery tank (3), synthetic reation kettle (1) and hydrolysis reaction cauldron (6), the feed end of decompression stills (7) and the discharge end intercommunication of hydrolysis reaction cauldron (6), the distillation end of decompression stills (7) and the feed end intercommunication of second condenser (8), the condensation end of second condenser (8) is connected on finished product jar (9), the evacuation end of vacuum system (10) is connected on finished product jar (9).

2. The system for rapidly synthesizing propiophenone from a pharmaceutical intermediate according to claim 1, wherein the cooling layers of the first condenser (2) and the second condenser (8) are connected to a water circulation line (16).

3. The system for rapidly synthesizing propiophenone from a pharmaceutical intermediate according to claim 1, wherein the pipelines in the walls of the synthesis reactor (1) and the hydrolysis reactor (6) are connected to an ice maker pipeline (14).

4. The system for rapidly synthesizing propiophenone from a pharmaceutical intermediate according to claim 2, wherein the water circulation line (16) is connected to the water circulation system (11).

5. A system for the rapid synthesis of propiophenone from a pharmaceutical intermediate according to claim 3, wherein the ice maker conduit (14) is connected to an ice maker system (13).

6. The system for rapidly synthesizing propiophenone from a pharmaceutical intermediate according to claim 1, wherein the heating line of the synthesis reactor (1) is in communication with a vapor line (17).

7. The system for rapidly synthesizing propiophenone from a pharmaceutical intermediate according to claim 6, wherein the vapor line (17) is in communication with a vapor heating system (12).

8. The system for rapidly synthesizing propiophenone from a pharmaceutical intermediate according to claim 1, wherein the structure of the synthesis reactor (1) is as follows: the reaction kettle comprises a synthesis reaction kettle body (101), baffle plates (102), cooling pipes (103) and stirring blades (104), wherein the baffle plates (102) are vertically and uniformly distributed in the synthesis reaction kettle body (101), the cooling pipes (103) are vertically distributed in the synthesis reaction kettle body (101) in a plurality of annular arrangements, and the stirring blades (104) are arranged in the synthesis reaction kettle body (101) from top to bottom.