CN211199073U

CN211199073U - Synthesis device of m-bromonitrobenzene

Info

Publication number: CN211199073U
Application number: CN201821576089.6U
Authority: CN
Inventors: 王丽君
Original assignee: Zibo Vocational Institute
Current assignee: Zibo Vocational Institute
Priority date: 2018-09-26
Filing date: 2018-09-26
Publication date: 2020-08-07
Anticipated expiration: 2028-09-26

Abstract

The utility model belongs to the chemical industry equipment field, concretely relates to synthesizer of m-bromonitrobenzene. The reactor comprises a reactor, water vapor cauldron and distillation column, the reactor is connected and is connected the water vapor cauldron, the bottom of water vapor cauldron sets up the steam chamber, the steam chamber is located the inside of water vapor cauldron, the top in steam chamber sets up a plurality of nozzles towards the top, nitrobenzene jar and drying tower are connected respectively to the top export of water vapor cauldron, set up first valve on the pipeline between water vapor cauldron and the nitrobenzene jar, set up the second valve on the pipeline between water vapor cauldron and the drying tower, be equipped with the heat exchanger on the pipeline between water vapor cauldron and the drying tower, heat exchanger access connection water storage tank, heat exchanger exit linkage heater, heater exit linkage steam chamber import, the exit linkage distillation column of drying tower, distillation column tower liftout gate passes through pipe connection product collection tank. The utility model discloses production efficiency is high, and the energy consumption is low, and is with low costs, resources are saved, and the m-bromonitrobenzene purity and the yield that obtain are high.

Description

Synthesis device of m-bromonitrobenzene

Technical Field

The utility model belongs to the chemical industry equipment field, concretely relates to synthesizer of m-bromonitrobenzene.

Background

The m-bromonitrobenzene is light yellow needle-shaped crystal, is easy to dissolve in ethanol, is soluble in ether and benzene, and is insoluble in water. Is toxic. Used as an organic synthesis intermediate, used for synthesizing m-bromoaniline and m-bromothiophenol in the pharmaceutical industry and producing the antiemetic, namely hypnotic, sedative and antiemetic.

The prior art processes for preparation are generally obtained by bromination of nitrobenzene. Firstly putting nitrobenzene, iron powder and carbon tetrachloride into a reaction kettle, heating to 120 ℃, dropwise adding bromine, finishing the addition within 2 hours, then supplementing the iron powder and the bromine twice at the temperature of 120 plus 135 ℃, and carrying out heat preservation and stirring to obtain a finished product. However, the process has high energy consumption and cost, and the purity of the obtained m-bromonitrobenzene also needs to be further improved. However, the prior art does not describe a m-bromonitrobenzene synthesis apparatus.

Disclosure of Invention

To prior art's not enough, the utility model aims at providing a synthesizer of m-bromonitrobenzene, production efficiency is high, and the energy consumption is low, and is with low costs, resources are saved, and the m-bromonitrobenzene purity and the yield that obtain are high.

The utility model relates to a m-bromonitrobenzene synthesis device, which comprises a reactor, the device comprises a water steaming kettle and a distillation tower, an inlet connection feed line on the upper part of the reactor, an outlet at the bottom of the reactor is connected with the inlet of the water steaming kettle, a feed inlet is arranged on the wall of the upper part of the water steaming kettle, the bottom of the water steaming kettle is provided with a steam cavity, the steam cavity is positioned in the water steaming kettle, a plurality of nozzles are arranged at the top of the steam cavity towards the upper part, a top outlet of the water steaming kettle is connected with a nitrobenzene tank and a drying tower through a pipeline respectively, a first valve is arranged on the pipeline between the water steaming kettle and the nitrobenzene tank, a second valve is arranged on the pipeline between the water steaming kettle and the drying tower, a heat exchanger inlet connection water storage tank is arranged at the heat exchanger, a heater outlet connection heater is arranged at the steam cavity, an outlet connection distillation tower.

A condenser is arranged on a pipeline between the distillation tower and the product collecting tank.

A pump is arranged on the pipeline between the heater and the steam cavity.

5-20 nozzles are arranged on the top of the steam cavity facing upwards and are uniformly distributed.

The outlet of the nitrobenzene tank is connected with a feed line.

The utility model discloses material transmission between each equipment is preferred to be provided power by the pump.

The operation process comprises the following steps: adding nitrobenzene, iron powder and liquid bromine as reaction raw materials into a reactor through feed pipelines respectively, and adding bromine under a heating condition to perform reaction. And (3) the material after the reaction enters a water evaporation kettle, a saturated solution of water and sodium sulfite is added into the water evaporation kettle from a feeding hole, water vapor distillation is carried out in the water evaporation kettle, the first valve is opened, the second valve is closed, unreacted nitrobenzene is evaporated out firstly and enters a nitrobenzene tank to be collected, and nitrobenzene in the nitrobenzene tank returns to a feeding pipeline for secondary reaction, so that the cost is reduced, and the resource is saved. Then the first valve is closed, the second valve is opened, the organic material is evaporated out along with the steam, the organic material enters a drying tower for drying after heat exchange through a heat exchanger, water in a water storage tank exchanges heat in the heat exchanger, the organic material is cooled and condensed, meanwhile, heat is absorbed to become warm water, and then the warm water enters a heater for heating until the water is boiled and then enters a steam cavity at the bottom of a steam kettle. The steam chamber is located the inside of steam kettle, and the top in steam chamber sets up a plurality of nozzles towards the top, and inside steam kettle was spouted by the nozzle through the steam chamber, fully contacted with the material, and it is effectual to evaporate, improves product purity. And (3) distilling the dried material in the drying tower in a distillation tower, collecting fractions, condensing the fractions by a condenser, and collecting the fractions in a product collection tank to obtain the m-bromonitrobenzene.

Compared with the prior art, the utility model has the advantages of it is following:

(1) the utility model discloses a synthesizer of m-bromonitrobenzene, production efficiency is high, the m-bromonitrobenzene purity and the yield that obtain are high.

(2) The utility model discloses set up the heat exchanger between water evaporation cauldron and drying tower, the heat of the material that comes out from the water evaporation cauldron is fully absorbed to water, in getting into the water evaporation cauldron again after the heating, heat recovery, energy saving consumed the festival.

(3) The utility model discloses set up the steam chamber in the bottom of steam kettle, the top in steam chamber sets up a plurality of nozzles towards the top, and inside vapor was spouted by the nozzle to steam kettle through the steam chamber, with the material fully contact, steam is effectual, can improve the purity of product, and the product purity that the preparation obtained is high.

(4) The utility model discloses evaporate unreacted nitrobenzene, get into and collect in the nitrobenzene jar, return the feed line and react once more, reduce cost, resources are saved.

Drawings

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

in the figure: 1-feeding pipeline, 2-reactor, 3-nitrobenzene tank, 4-first valve, 5-second valve, 6-heat exchanger, 7-water storage tank, 8-drying tower, 9-condenser, 10-product collecting tank, 11-distillation tower, 12-heater, 13-pump, 14-steam cavity, 15-nozzle, 16-water steaming kettle and 17-feeding hole.

Detailed Description

The present invention will be further described with reference to the following examples.

Examples

A m-bromonitrobenzene synthesis device is shown in figure 1 and comprises a reactor 2, a water evaporation kettle 16 and a distillation tower 11, wherein an inlet at the upper part of the reactor 2 is connected with a feeding pipeline 1, an outlet at the bottom of the reactor 2 is connected with an inlet of the water evaporation kettle 16, a feeding hole 17 is arranged on the wall of the upper part of the water evaporation kettle 16, a steam cavity 14 is arranged at the bottom of the water evaporation kettle 16, the steam cavity 14 is positioned inside the water evaporation kettle 16, a plurality of nozzles 15 are arranged towards the upper part of the top of the steam cavity 14, an outlet at the top of the water evaporation kettle 16 is respectively connected with a nitrobenzene tank 3 and a drying tower 8 through pipelines, a first valve 4 is arranged on the pipeline between the water evaporation kettle 16 and the nitrobenzene tank 3, a second valve 5 is arranged on the pipeline between the water evaporation kettle 16 and the drying tower 8, a heat exchanger 6 is arranged on the pipeline between the water evaporation kettle 16 and the drying tower 8, an inlet of the heat exchanger 6 is connected, the outlet of the heater 12 is connected with the inlet of the steam cavity 14, the outlet of the drying tower 8 is connected with the distillation tower 11, and the outlet at the top of the distillation tower 11 is connected with the product collecting tank 10 through a pipeline.

A condenser 9 is provided on the pipe between the distillation column 11 and the product collection tank 10.

A pump 13 is provided on the conduit between the heater 12 and the steam chamber 14.

The top of the steam chamber 14 is provided with 5-20 nozzles 15 facing upwards.

The outlet of the nitrobenzene tank 3 is connected with a feed line 1.

The operation process comprises the following steps: nitrobenzene, iron powder and liquid bromine which are used as reaction raw materials are respectively added into a reactor 2 through a feed pipeline 1, and bromine is added under the heating condition for reaction. The material after the reaction enters the water evaporation kettle 16, saturated solution of water and sodium sulfite is added into the water evaporation kettle 16 through the feed inlet 17, steam distillation is carried out in the water evaporation kettle 16, the first valve 4 is opened, the second valve 5 is closed, unreacted nitrobenzene is evaporated out firstly and enters the nitrobenzene tank 3 for collection, and nitrobenzene in the nitrobenzene tank 3 returns to the feed pipeline 1 for reaction again, so that the cost is reduced, and the resources are saved. Then the first valve 4 is closed, the second valve 5 is opened, the organic material is steamed out along with the steam, the organic material enters a drying tower 8 for drying after heat exchange through a heat exchanger 6, water in a water storage tank 7 exchanges heat in the heat exchanger 6, the organic material is cooled and condensed, meanwhile, heat is absorbed to become warm water, and then the warm water enters a heater 12 for heating until the warm water is boiled and then enters a steam cavity 14 at the bottom of a steam kettle 16. Steam chamber 14 is located the inside of steam kettle 16, and the top of steam chamber 14 sets up a plurality of nozzles 15 towards the top, and steam is inside steam kettle 16 by nozzle 15 spouts through steam chamber 14, fully contacts with the material, and it is effectual to evaporate water, improves product purity. And (3) feeding the dried material in the drying tower 8 into a distillation tower 11 for distillation, collecting fractions, condensing the fractions by a condenser 9, and feeding the fractions into a product collecting tank 10 for collection to obtain the m-bromonitrobenzene.

Claims

1. A synthetic device of m-bromonitrobenzene is characterized in that: comprises a reactor (2), a water vapor kettle (16) and a distillation tower (11), wherein an inlet at the upper part of the reactor (2) is connected with a feeding pipeline (1), an outlet at the bottom of the reactor (2) is connected with an inlet of the water vapor kettle (16), a feeding hole (17) is arranged on the wall of the upper part of the water vapor kettle (16), a steam cavity (14) is arranged at the bottom of the water vapor kettle (16), the steam cavity (14) is positioned inside the water vapor kettle (16), a plurality of nozzles (15) are arranged towards the upper part of the top of the steam cavity (14), the outlet at the top of the water vapor kettle (16) is respectively connected with a nitrobenzene tank (3) and a drying tower (8) through a pipeline, a first valve (4) is arranged on the pipeline between the water vapor kettle (16) and the nitrobenzene tank (3), a second valve (5) is arranged on the pipeline between the water vapor kettle (16) and the drying tower (8), and a heat exchanger (6) is arranged on the pipeline between the water vapor kettle (, the inlet of the heat exchanger (6) is connected with the water storage tank (7), the outlet of the heat exchanger (6) is connected with the heater (12), the outlet of the heater (12) is connected with the inlet of the steam cavity (14), the outlet of the drying tower (8) is connected with the distillation tower (11), and the outlet of the top of the distillation tower (11) is connected with the product collecting tank (10) through a pipeline.

2. The apparatus for synthesizing m-bromonitrobenzene according to claim 1, wherein: a condenser (9) is arranged on a pipeline between the distillation tower (11) and the product collecting tank (10).

3. The apparatus for synthesizing m-bromonitrobenzene according to claim 1, wherein: a pump (13) is arranged on a pipeline between the heater (12) and the steam cavity (14).

4. The apparatus for synthesizing m-bromonitrobenzene according to claim 1, wherein: 5-20 nozzles (15) are arranged on the top of the steam cavity (14) facing upwards.

5. The apparatus for synthesizing m-bromonitrobenzene according to claim 1, wherein: the outlet of the nitrobenzene tank (3) is connected with a feed pipeline (1).