CN210340729U

CN210340729U - Continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane

Info

Publication number: CN210340729U
Application number: CN201920466633.XU
Authority: CN
Inventors: 胡国宜; 胡锦平; 张培锋; 黄磊
Original assignee: Changzhou Sunlight Pharmaceutical Co ltd
Current assignee: Changzhou Sunlight Pharmaceutical Co ltd
Priority date: 2019-04-08
Filing date: 2019-04-08
Publication date: 2020-04-17
Anticipated expiration: 2029-04-08

Abstract

The utility model discloses a continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane, which comprises a continuous flow reactor, a heat exchanger, a crystallizing tank, a dripping tank and a centrifuge; a feed inlet and a discharge outlet are arranged on the continuous flow reactor; a feed inlet and a discharge outlet are arranged on the heat exchanger; a feed inlet, a dropping port and a discharge port are arranged on the crystallizing tank; a feed inlet, a discharge outlet and an exhaust outlet are arranged on the dripping tank; a feed inlet and a mother liquor outlet are arranged on the centrifugal machine; the discharge hole of the continuous flow reactor is directly connected with the feed inlet of the heat exchanger; the discharge hole of the heat exchanger is connected with the feed inlet of the crystallizing tank through a back pressure valve; the discharge hole of the dripping tank is directly connected with the dripping port of the crystallizing tank; the discharge port of the crystallizing tank is directly connected with the feed port of the centrifuge. The utility model discloses continuous flow reaction system production efficiency is high, and the reaction is single, and product purity is high, and the security is high, and the raw materials consumption is few, and the wastes material discharges fewly, and is friendly to the environment.

Description

Continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane

Technical Field

The utility model relates to a continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane.

Background

Nitration is a common chemical reaction unit process, and is a reaction that introduces nitro groups into organic compound molecules. In the chemical development process, the strong polarity of the nitro group is utilized to endow the compound with certain functions, such as deepening the color of the dye, improving the reaction activity of the compound and the like, and the nitro group can also be used for synthesizing compounds such as amino compounds and the like. Nitration requires maintaining appropriate reaction conditions to avoid side reactions such as polynitrogen formation and oxidation. Nitration is an exothermic reaction and the reaction rate is fast and poorly controlled, leading to explosions.

The compound 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane is mainly applied to production of semiconductor IC chip protective films, metal interlayer insulating materials of multi-chip modules MCM-D, flexible printed circuit boards FPC, high-grade electronic packaging materials and the like, and has good market prospect. The traditional method for preparing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane uses bisphenol AF as a main raw material and nitric acid as a nitration reagent, and carries out nitration reaction in an intermittent reaction kettle, so that the reaction safety is poor, the pollution is heavy, and the product quality is not high.

To date, no report has been made on the production of 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane in a continuous flow reactor.

SUMMERY OF THE UTILITY MODEL

The utility model aims at solving the above problem and providing a continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane.

Realize the utility model discloses the technical scheme of purpose is: a continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane comprises a continuous flow reactor, a heat exchanger, a crystallizing tank, a dripping tank and a centrifuge; a feeding hole and a discharging hole are arranged on the continuous flow reactor; a feed inlet and a discharge outlet are arranged on the heat exchanger; the crystallizing tank is provided with a feed inlet, a dropping port and a discharge port; the dripping tank is provided with a feed inlet, a discharge outlet and an exhaust port; a feed inlet and a mother liquor outlet are arranged on the centrifugal machine; the discharge hole of the continuous flow reactor is directly connected with the feed inlet of the heat exchanger; the discharge hole of the heat exchanger is connected with the feed hole of the crystallizing tank through a back pressure valve; the discharge hole of the dripping tank is directly connected with the dripping hole of the crystallizing tank; and the discharge hole of the crystallization tank is directly connected with the feed inlet of the centrifuge.

The utility model discloses a continuous flow reaction system for producing 2,2' -two [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane still includes metering components; the metering assembly consists of a first metering pump, a second metering pump, a first flow meter and a second flow meter; the first metering pump and the first flowmeter are connected in series on the same pipeline, and the second metering pump and the second flowmeter are connected in series on another pipeline; the two pipes are connected in parallel with the feed inlet of the continuous flow reactor.

The utility model discloses positive effect that has: the utility model discloses continuous flow reaction system production efficiency is high, and the reaction is single, and almost no trinitration product produces, and product purity is high, and reaction and heat transfer are rapid, and the security is high, and the raw materials consumption is few, and the wastes material discharges fewly, and is friendly to the environment.

Drawings

Fig. 1 is a schematic diagram of a continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane according to the present invention.

Detailed Description

(example 1)

Referring to fig. 1, the continuous flow reaction system for producing 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane of the present example includes a continuous flow reactor 1, a heat exchanger 2, a crystallization tank 3, a dropping tank 4, a centrifuge 5, a back pressure valve 6, and a metering assembly.

The continuous flow reactor 1 is provided with a continuous flow reactor feed inlet 11 and a continuous flow reactor discharge outlet 12, the heat exchanger 2 is provided with a heat exchanger feed inlet 21 and a heat exchanger discharge outlet 22, the crystallizer 3 is provided with a crystallizer feed inlet 31, a dropping port 32 and a crystallizer discharge outlet 33, the dropping tank 4 is provided with a dropping tank feed inlet 41, a dropping tank discharge outlet 42 and a dropping tank exhaust outlet 43, and the centrifuge 5 is provided with a centrifuge feed inlet 51 and a mother liquor outlet 52.

The continuous flow reactor discharge port 12 of the continuous flow reactor 1 is directly connected with the heat exchanger feed port 21 of the heat exchanger 2, the heat exchanger discharge port 22 of the heat exchanger 2 is connected with the crystallizer feed port 31 of the crystallizer 3 through the back pressure valve 6, the dropping tank discharge port 42 of the dropping tank 4 is directly connected with the dropping port 32 of the crystallizer 3, and the crystallizer discharge port 33 of the crystallizer 3 is directly connected with the centrifuge feed port 51 of the centrifuge 5.

The metering assembly consists of a first metering pump 71-1, a second metering pump 71-2, a first flow meter 72-1 and a second flow meter 72-2; the first metering pump 71-1 and the first flowmeter 72-1 are connected in series on the same pipeline, and the second metering pump 71-2 and the second flowmeter 72-2 are connected in series on another pipeline; the two pipes are connected in parallel to the continuous flow reactor feed port 11 of the continuous flow reactor 1.

The process comprises the following steps: dissolving a main raw material bisphenol AF in acetic acid, then entering a continuous flow reactor 1 through a first metering pump 71-1 and a first flow meter 72-1, meanwhile, entering nitric acid into the continuous flow reactor 1 through a second metering pump 71-2 and a second flow meter 72-2, mixing and reacting in the continuous flow reactor 1 by controlling the molar ratio of the bisphenol AF to the nitric acid through flow control, continuously passing through a series of mass transfer enhancement micro-channel modules and a straight-flow micro-channel module, cooling through a heat exchanger 2 after the reaction is finished, entering a crystallization tank 3, adding water into the crystallization tank 3 through a dropping tank 4 to crystallize the material, and finally filtering through a centrifuge 5 to obtain the product.

Claims

1. A continuous flow reaction system for the production of 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane characterized by: comprises a continuous flow reactor (1), a heat exchanger (2), a crystallizing tank (3), a dripping tank (4) and a centrifuge (5);

a continuous flow reactor feeding port (11) and a continuous flow reactor discharging port (12) are arranged on the continuous flow reactor (1);

a heat exchanger feed port (21) and a heat exchanger discharge port (22) are formed in the heat exchanger (2);

a crystallizer feed inlet (31), a dropping port (32) and a crystallizer discharge outlet (33) are formed in the crystallizer (3);

a feeding hole (41) of the dripping tank, a discharging hole (42) of the dripping tank and an exhaust port (43) of the dripping tank are arranged on the dripping tank (4);

a centrifuge feed inlet (51) and a mother liquor outlet (52) are formed in the centrifuge (5);

the continuous flow reactor discharge port (12) of the continuous flow reactor (1) is directly connected with the heat exchanger feed port (21) of the heat exchanger (2);

a heat exchanger discharge hole (22) of the heat exchanger (2) is connected with a crystallizer feed hole (31) of the crystallizer (3) through a back pressure valve (6);

a discharge port (42) of the dripping tank (4) is directly connected with a dripping port (32) of the crystallizing tank (3);

and a crystallizing tank discharge port (33) of the crystallizing tank (3) is directly connected with a centrifuge feed port (51) of the centrifuge (5).

2. A continuous flow reaction system for the production of 2,2' -bis [ (3-nitro-4-hydroxy) phenyl ] hexafluoropropane as claimed in claim 1 wherein: the system also includes a metering assembly;

the metering assembly consists of a first metering pump (71-1), a second metering pump (71-2), a first flow meter (72-1) and a second flow meter (72-2); the first metering pump (71-1) and the first flow meter (72-1) are connected in series on the same pipeline, and the second metering pump (71-2) and the second flow meter (72-2) are connected in series on another pipeline; the two pipelines are connected in parallel with the continuous flow reactor feed inlet (11) of the continuous flow reactor (1).