CN210449153U - System for realizing coupling reaction - Google Patents
System for realizing coupling reaction Download PDFInfo
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- CN210449153U CN210449153U CN201921029256.XU CN201921029256U CN210449153U CN 210449153 U CN210449153 U CN 210449153U CN 201921029256 U CN201921029256 U CN 201921029256U CN 210449153 U CN210449153 U CN 210449153U
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Abstract
The utility model relates to a chemical industry equipment technical field. The utility model discloses a system for realizing coupling reaction, which comprises a reactant system, a coupling reaction kettle, a product collecting tank, a coupling condenser and a coupling explosion venting tank; the reaction system comprises a soft water tank, a carbonate solution tank, a raw material liquid storage tank, a halogenated nitrobenzene storage tank, a high-purity nitrogen tank and a catalyst feeding bin, wherein a discharge hole in the bottom of the coupling reaction kettle is connected with a product collecting tank; a circulating cooling pipeline is arranged on the outer side of the coupling reaction kettle and is connected with a circulating cooling water return device of a circulating cooling water upper water device; the coupling condenser is connected with the coupling reaction kettle; the coupling condenser is connected with the cooling water upper water tank and the cooling water return tank and is connected with the vent pipe; the coupling explosion venting tank is connected with the top of the coupling reaction kettle. The utility model discloses can realize the high efficiency of coupling reaction under the minimum condition of consumption and go on, wherein the yield of result is up to 97%, and the yield of hydrochloride is up to 94.7%.
Description
Technical Field
The utility model belongs to the technical field of the chemical industry equipment technique and specifically relates to a system for realize coupling reaction is related to.
Background
In the process of synthesizing the phenylamine compounds, the coupling reaction of the phenylboronic acid compounds and the chloronitrobenzene is an important step, and the coupling reaction of the phenylboronic acid compounds, the chloroaniline and the carbonate is generally adopted under the action of a catalyst. In the whole process, not only the target product needs to be efficiently synthesized, but also the recovery of byproducts and some recycled reaction reagents can be realized; in the prior art, a complete reaction system for coupling reaction of phenylboronic acid compounds and chloroaniline in the synthesis process of phenylamine compounds does not exist, and a corresponding efficient reaction system is required along with the increase of the demand of corresponding products.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem, the utility model provides a can realize high-efficient phenylboronic acid compound and halogenated nitrobenzene class coupling reaction and can realize the coupling reaction system that reactant and accessory substance were retrieved.
In order to achieve the above object, the utility model adopts the following technical scheme:
a system for carrying out a coupling reaction, comprising:
the system comprises a reactant system, a coupling reaction kettle, a product collecting tank, a coupling condenser and a coupling explosion venting tank;
the reaction system comprises a soft water tank, a carbonate solution tank, a raw material liquid storage tank, a halogenated nitrobenzene storage tank, a high-purity nitrogen tank and a catalyst feeding bin, wherein the soft water tank, the carbonate solution tank, the raw material liquid storage tank and the halogenated nitrobenzene storage tank are respectively connected with a switch valve and then are respectively connected with the tops of the coupling reaction kettles, the soft water tank is connected with the top of the catalyst feeding bin, the bottom of the catalyst feeding bin is connected with the top of the coupling reaction kettle, the catalyst feeding bin is connected with a common nitrogen tank, the common nitrogen tank is also connected with the top of the coupling reaction kettle, and the catalyst feeding bin is connected with an emptying pipe; a solid feeding port is arranged at the top of the catalyst feeding bin; the high-purity nitrogen tank is connected to the top of the coupling reaction kettle;
a discharge port at the bottom of the coupling reaction kettle is connected with a product collecting tank through a switch valve, a control valve, a coupling reaction liquid transfer pump and a check valve in sequence;
a circulating cooling pipeline is arranged outside the coupling reaction kettle and is connected with a circulating cooling water feeding device consisting of a cooling water feeding tank and a steam condensate tank and a circulating cooling water returning device consisting of a cooling water returning tank and a low-pressure steam tank;
a condensate outlet of the coupling condenser is connected with the top of the coupling reaction kettle through a switch valve, and the top of the coupling reaction kettle is connected with a gas inlet of the coupling condenser through the switch valve; the cooling water inlet of the coupling condenser is connected with a cooling water upper water tank, the cooling water outlet of the coupling condenser is connected with a cooling water return tank, and the coupling condenser is connected with an emptying pipe;
the coupling explosion venting tank is connected with the top of the coupling reaction kettle through an angle type safety valve, and is also connected with a pressure gauge, a liquid level gauge, an emergency leakage pipe and an explosion venting tank air outlet respectively.
The utility model discloses coupling reaction system's production process mainly is, carries out the mixed reaction with phenylboronic acid class compound, chloronitrobenzene and carbonate and generates phenylboronic acid nitro compound and retrieve the hydrochloride accessory substance, and its main process is to react phenylboronic acid class compound, chloronitrobenzene, carbonate, water and catalyst mixture weather under 85 degrees centigrade 0.25MPa pressure, and the qualified back cooling purification of curve obtains result and accessory substance.
Preferably, a switch valve and a control valve are arranged between the soft water tank and the top of the catalyst feeding bin; a check valve and a switch valve are sequentially arranged between the common nitrogen tank and the catalyst feeding bin; a switch valve and a needle valve connected with a pressure indicator are arranged between the catalyst feeding bin and the emptying pipe; a switch valve is arranged between the common nitrogen tank and the top of the coupling reaction kettle; a check valve and a switch valve are arranged between the high-purity nitrogen tank and the top of the coupling reaction kettle at one time; a control valve is arranged between the catalyst feeding bin and the top of the coupling reaction kettle.
Preferably, a needle valve and a switch valve which are connected with a pressure indicator are arranged between the cooling water upper water tank and the circulating cooling pipeline; a switch valve is arranged between the steam condensate tank and the circulating cooling pipeline.
Preferably, a switch valve, a needle valve connected with a pressure indicator and a temperature indicator are arranged between the cooling water return tank and the circulating cooling pipeline; and a temperature valve, a flow pore plate connected with the flow indicator, a switch valve, a needle valve connected with the pressure indicator and a temperature indicator are also arranged between the low-pressure steam tank and the circulating cooling pipeline.
Preferably, a control valve connected with a pressure indicator is arranged between the gas inlet of the coupling condenser and the top of the coupling reaction kettle; a switch valve and a flow orifice plate connected with a flow indicator are sequentially arranged between the cooling water upper water tank and the cooling water inlet of the coupling condenser; a switch valve is arranged between the cooling water return tank and the cooling water outlet of the coupling condenser; a switch valve is arranged between the coupling condenser and the emptying pipe.
Preferably, the two ends of the switch valve between the coupling condenser and the emptying pipe are connected with an oxygen content tester in parallel.
Preferably, the coupling explosion venting tank is also connected with the top of the coupling reaction kettle through two pressure type rupture discs, and a needle valve connected with a pressure indicator is arranged between the two pressure type rupture discs.
Preferably, a stirring paddle is arranged in the coupling reaction kettle and connected with a motor at the top of the coupling reaction kettle; the coupling reaction kettle is provided with a temperature indicator, a pressure indicator and a liquid level indicator.
Preferably, the system for realizing the coupling reaction is also provided with a vent cap, and the vent cap is connected with the waste gas pipe after being connected with the butterfly valve.
Preferably, the coupling condenser and the coupling reaction kettle are provided with heat insulation layers on the outer sides.
The utility model discloses in connect through corresponding material pipeline or through the electricity between each device.
Therefore, the utility model discloses following beneficial effect has: the utility model can realize the high-efficiency proceeding of the coupling reaction under the condition of consuming the least raw materials, and can recover the by-product (mainly hydrochloride) as much as possible; wherein the yield of the product (the benzene nitro compound) is as high as 97 percent, and the yield of the hydrochloride is as high as 94.7 percent.
Drawings
FIG. 1 is a schematic diagram of a coupling reaction system realized in example 1;
FIG. 2 is a schematic diagram of a coupling reaction system realized in example 2;
in the figure: a reactant system 1, a soft water tank 11, a carbonate solution tank 12, a raw material liquid storage tank 13, a halogenated nitrobenzene storage tank 14, a high-purity nitrogen tank 15, a catalyst feeding bin 16, a common nitrogen tank 17, a high-purity nitrogen tank 18, a solid feeding port 19, a coupling reaction kettle 2, a coupling reaction liquid transfer pump 21, a stirring paddle 22, a motor 23, a circulating cooling pipeline 24, a product collecting tank 3, a coupling condenser 4, a condensate outlet 41, a gas inlet 42, a cooling water inlet 43, a cooling water outlet 44, a coupling explosion venting tank 5, an explosion venting tank gas outlet 51, a circulating cooling water upper water device 61, a cooling water upper water 62, a steam condensate tank 63, a circulating cooling water return device 64, a cooling water return water tank 65, a low-pressure steam tank 66, a pressure indicator 71, a temperature indicator 72, a flow indicator 73, an oxygen content determinator 74, a pressure gauge 75, a liquid level meter 76 and a liquid level indicator 77, a vent pipe 80, an emergency vent pipe 81, a vent cap 82, an exhaust pipe 83, a heat insulation layer 84, a switch valve 90, a control valve 91, a check valve 92, a needle valve 93, a temperature valve 94, a flow orifice plate 95, an angle type safety valve 96, a pressure type rupture disk 97 and a butterfly valve 98.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
It is obvious that the described embodiments are only some of the embodiments of the present invention, and not all of them. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
In the present invention, all the devices and materials are commercially available or commonly used in the industry, and the devices are connected or electrically connected by corresponding material pipes, and the methods in the following embodiments are conventional methods in the art unless otherwise specified.
Example 1
As shown in fig. 1, a system for realizing coupling reaction includes a reactant system 1, a coupling reaction kettle 2, a product collection tank 3, a coupling condenser 4 and a coupling explosion venting tank 5;
the reaction system comprises a soft water tank 11, a carbonate solution tank 12, a raw material liquid storage tank 13, a halogenated nitrobenzene storage tank 14, a high-purity nitrogen tank 15 and a catalyst feeding bin 16, wherein the soft water tank, the carbonate solution tank, the raw material liquid storage tank and the halogenated nitrobenzene storage tank are respectively connected with a switch valve 90 and then are connected with the tops of the coupling reaction kettles 2 respectively; the soft water tank is connected with the top of the catalyst feeding bin 16 through a switch valve 90 and a control valve 91 in sequence; the catalyst feeding bin 16 is connected with the common nitrogen tank 17, and a check valve 92 and a switch valve 90 are sequentially arranged between the common nitrogen tank 17 and the catalyst feeding bin 16; the bottom of the catalyst feeding bin 16 is connected with the top of the coupling reaction kettle 2 through a control valve 91; the common nitrogen tank 17 is also directly connected with the top of the coupling reaction kettle 2 through a switch valve 90; the catalyst feeding bin 16 is connected with an emptying pipe 80, and a switch valve 90 and a needle valve 93 connected with a pressure indicator 71 are arranged between the catalyst feeding bin 16 and the emptying pipe 80; the high-purity nitrogen tank 18 is connected to the top of the coupling reaction kettle 2, and a check valve 92 and a switch valve 90 are sequentially arranged between the high-purity nitrogen tank 18 and the top of the coupling reaction kettle 2; the top of the catalyst feeding bin is provided with a solid feeding port 19;
a discharge hole at the bottom 2 of the coupling reaction kettle is connected with a product collecting tank 3 through a switch valve 90, a control valve 91, a coupling reaction liquid transferring pump 21 and a check valve 92 in sequence; a stirring paddle 22 is arranged in the coupling reaction kettle and is connected with a motor 23 at the top of the coupling reaction kettle; the coupling reaction kettle is provided with a temperature indicator 72, a pressure indicator 71 and a liquid level indicator 77; a circulating cooling pipeline 24 is arranged on the outer side of the coupling reaction kettle and is connected with a circulating cooling water upper water device 61 consisting of a cooling water upper water tank 62 and a steam condensate water tank 63 and a circulating cooling water return device 64 consisting of a cooling water return tank 65 and a low-pressure steam tank 66; a needle valve 93 and a switch valve 90 which are connected with the pressure indicator 71 are arranged between the cooling water upper water tank and the circulating cooling pipeline; a switch valve 90 is arranged between the steam condensate tank and the circulating cooling pipeline; a switch valve 90, a needle valve 93 connected with the pressure indicator 71 and a temperature indicator 72 are arranged between the cooling water return tank and the circulating cooling pipeline; a temperature valve 94, a flow orifice plate 95 connected with the flow indicator 73, a switch valve 90, a needle valve 93 connected with the pressure indicator 71 and a temperature indicator 72 are arranged between the low-pressure steam tank and the circulating cooling pipeline;
a condensate outlet 41 of the coupling condenser 4 is connected with the top of the coupling reaction kettle 2 through a switch valve 90, and the top of the coupling reaction kettle is connected with a gas inlet 42 of the coupling condenser through the switch valve 90; a cooling water inlet 43 of the coupling condenser is connected with a cooling water upper water tank 62, a cooling water outlet 44 of the coupling condenser is connected with a cooling water return tank 65, and the coupling condenser 4 is connected with a vent pipe 80; a control valve 91 connected with the pressure indicator 71 is arranged between the gas inlet 42 of the coupling condenser and the top of the coupling reaction kettle 2; a switch valve 90 and a flow orifice plate 95 connected with a flow indicator 73 are sequentially arranged between the cooling water upper water tank 62 and the cooling water inlet 43 of the coupling condenser; a switch valve 90 is arranged between the cooling water return tank 65 and the cooling water outlet 44 of the coupling condenser; a switch valve 90 is arranged between the coupling condenser 4 and the emptying pipe 80; the two ends of the switch valve 90 between the coupling condenser 4 and the emptying pipe 80 are connected with the oxygen content tester 74 in parallel;
the coupling explosion venting tank 5 is connected with the top of the coupling reaction kettle 2 through an angle type safety valve 96, and is also respectively connected with a pressure gauge 75, a liquid level gauge 76, an emergency relief pipe 81 and an explosion venting tank air outlet 51; the coupling explosion venting tank is also connected with the top of the coupling reaction kettle 2 through two pressure type rupture discs 97, and a needle valve 93 connected with a pressure indicator 71 is arranged between the two pressure type rupture discs.
The system for realizing the coupling reaction is also provided with a vent cap 82, and the vent cap is connected with a butterfly valve 98 and then connected with an exhaust pipe 83;
and a heat insulation layer 84 is arranged on the outer sides of the coupling condenser and the coupling reaction kettle.
Example 2
As shown in fig. 2, a system for realizing coupling reaction includes a reactant system 1, a coupling reaction kettle 2, a product collection tank 3, a coupling condenser 4 and a coupling explosion venting tank 5;
the reaction system comprises a soft water tank 11, a carbonate solution tank 12, a raw material liquid storage tank 13, a halogenated nitrobenzene storage tank 14, a high-purity nitrogen tank 15 and a catalyst feeding bin 16, wherein the soft water tank, the carbonate solution tank, the raw material liquid storage tank and the halogenated nitrobenzene storage tank are respectively connected with a switch valve 90 and then are connected with the tops of the coupling reaction kettles 2 respectively; the soft water tank is connected with the top of the catalyst feeding bin 16 through a switch valve 90 and a control valve 91 in sequence; the catalyst feeding bin 16 is connected with the common nitrogen tank 17, and a check valve 92 and a switch valve 90 are sequentially arranged between the common nitrogen tank 17 and the catalyst feeding bin 16; the bottom of the catalyst feeding bin 16 is connected with the top of the coupling reaction kettle 2 through a control valve 91; the common nitrogen tank 17 is also directly connected with the top of the coupling reaction kettle 2 through a switch valve 90; the catalyst feeding bin 16 is connected with an emptying pipe 80, and a switch valve 90 and a needle valve 93 connected with a pressure indicator 71 are arranged between the catalyst feeding bin 16 and the emptying pipe 80; the high-purity nitrogen tank 18 is connected to the top of the coupling reaction kettle 2, and a check valve 92 and a switch valve 90 are sequentially arranged between the high-purity nitrogen tank 18 and the top of the coupling reaction kettle 2; the top of the catalyst feeding bin is provided with a solid feeding port 19;
a discharge hole at the bottom 2 of the coupling reaction kettle is connected with a product collecting tank 3 through a switch valve 90, a control valve 91, a coupling reaction liquid transferring pump 21 and a check valve 92 in sequence; a stirring paddle 22 is arranged in the coupling reaction kettle and is connected with a motor 23 at the top of the coupling reaction kettle; a circulating cooling pipeline 24 is arranged on the outer side of the coupling reaction kettle and is connected with a circulating cooling water upper water device 61 consisting of a cooling water upper water tank 62 and a steam condensate water tank 63 and a circulating cooling water return device 64 consisting of a cooling water return tank 65 and a low-pressure steam tank 66; a needle valve 93 and a switch valve 90 which are connected with the pressure indicator 71 are arranged between the cooling water upper water tank and the circulating cooling pipeline; a switch valve 90 is arranged between the steam condensate tank and the circulating cooling pipeline; a switch valve 90, a needle valve 93 connected with the pressure indicator 71 and a temperature indicator 72 are arranged between the cooling water return tank and the circulating cooling pipeline; a temperature valve 94, a flow orifice plate 95 connected with the flow indicator 73, a switch valve 90, a needle valve 93 connected with the pressure indicator 71 and a temperature indicator 72 are arranged between the low-pressure steam tank and the circulating cooling pipeline;
a condensate outlet 41 of the coupling condenser 4 is connected with the top of the coupling reaction kettle 2 through a switch valve 90, and the top of the coupling reaction kettle is connected with a gas inlet 42 of the coupling condenser through the switch valve 90; a cooling water inlet 43 of the coupling condenser is connected with a cooling water upper water tank 62, a cooling water outlet 44 of the coupling condenser is connected with a cooling water return tank 65, and the coupling condenser 4 is connected with a vent pipe 80; a control valve 91 connected with the pressure indicator 71 is arranged between the gas inlet 42 of the coupling condenser and the top of the coupling reaction kettle 2; a switch valve 90 and a flow orifice plate 95 connected with a flow indicator 73 are sequentially arranged between the cooling water upper water tank 62 and the cooling water inlet 43 of the coupling condenser; a switch valve 90 is arranged between the cooling water return tank 65 and the cooling water outlet 44 of the coupling condenser; a switch valve 90 is arranged between the coupling condenser 4 and the emptying pipe 80;
the coupling explosion venting tank 5 is connected with the top of the coupling reaction kettle 2 through an angle type safety valve 96, and is also respectively connected with a pressure gauge 75, a liquid level gauge 76, an emergency leakage pipe 81 and an explosion venting tank air outlet 51.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are considered to be within the scope of the invention as defined by the following claims.
Claims (10)
1. A system for carrying out a coupling reaction, comprising:
the system comprises a reactant system, a coupling reaction kettle, a product collecting tank, a coupling condenser and a coupling explosion venting tank;
the reactant system comprises a soft water tank, a carbonate solution tank, a raw material liquid storage tank, a halogenated nitrobenzene storage tank, a high-purity nitrogen tank and a catalyst feeding bin, wherein the soft water tank, the carbonate solution tank, the raw material liquid storage tank and the halogenated nitrobenzene storage tank are respectively connected with a switch valve and then are respectively connected with the tops of the coupling reaction kettles, the soft water tank is connected with the tops of the catalyst feeding bin, the bottom of the catalyst feeding bin is connected with the tops of the coupling reaction kettles, the catalyst feeding bin is connected with a common nitrogen tank, the common nitrogen tank is also connected with the tops of the coupling reaction kettles, and the catalyst feeding bin is connected with an emptying pipe; the top of the catalyst feeding bin is provided with a solid feeding port; the high-purity nitrogen tank is connected to the top of the coupling reaction kettle;
a discharge hole at the bottom of the coupling reaction kettle is connected with a product collecting tank through a switch valve, a control valve, a coupling reaction liquid transferring pump and a check valve in sequence;
a circulating cooling pipeline is arranged outside the coupling reaction kettle and is connected with a circulating cooling water upper water device consisting of a cooling water upper water tank and a steam condensate tank and a circulating cooling water return device consisting of a cooling water return tank and a low-pressure steam tank;
a condensate outlet of the coupling condenser is connected with the top of the coupling reaction kettle through a switch valve, and the top of the coupling reaction kettle is connected with a gas inlet of the coupling condenser through the switch valve; the cooling water inlet of the coupling condenser is connected with a circulating cooling water upper water tank, the cooling water outlet of the coupling condenser is connected with a circulating cooling water return tank, and the coupling condenser is connected with a vent pipe;
the coupling explosion venting tank is connected with the top of the coupling reaction kettle through an angle type safety valve and is also connected with a pressure gauge, a liquid level gauge, an emergency release pipe and an explosion venting tank air outlet respectively.
2. A system for carrying out a coupling reaction according to claim 1, wherein:
a switch valve and a control valve are arranged between the soft water tank and the top of the catalyst feeding bin;
a check valve and a switch valve are sequentially arranged between the common nitrogen tank and the catalyst feeding bin;
a switch valve and a needle valve connected with a pressure indicator are arranged between the catalyst feeding bin and the emptying pipe;
a switch valve is also arranged between the general nitrogen tank and the top of the coupling reaction kettle;
a check valve and a switch valve are sequentially arranged between the high-purity nitrogen tank and the top of the coupling reaction kettle;
and a control valve is arranged between the catalyst feeding bin and the top of the coupling reaction kettle.
3. A system for carrying out a coupling reaction according to claim 1, wherein:
a needle valve and a switch valve which are connected with a pressure indicator are arranged between the cooling water upper water tank and the circulating cooling pipeline;
and a switch valve is arranged between the steam condensate tank and the circulating cooling pipeline.
4. A system for carrying out a coupling reaction according to claim 1, wherein:
a switch valve, a needle valve connected with a pressure indicator and a temperature indicator are arranged between the cooling water return tank and the circulating cooling pipeline;
and a temperature valve, a flow pore plate connected with the flow indicator, a switch valve, a needle valve connected with the pressure indicator and a temperature indicator are also arranged between the low-pressure steam tank and the circulating cooling pipeline.
5. A system for carrying out a coupling reaction according to claim 1, wherein:
a control valve connected with a pressure indicator is arranged between the gas inlet of the coupling condenser and the top of the coupling reaction kettle;
a switch valve and a flow orifice plate connected with a flow indicator meter are sequentially arranged between the circulating cooling water upper water tank and the cooling water inlet of the coupling condenser; a switch valve is arranged between the circulating cooling water return tank and the cooling water outlet of the coupling condenser; and a switch valve is arranged between the coupling condenser and the emptying pipe.
6. A system for carrying out a coupling reaction according to claim 5, wherein:
and two ends of a switch valve between the coupling condenser and the emptying pipe are connected with an oxygen content tester in parallel.
7. A system for carrying out a coupling reaction according to claim 1, wherein:
the coupling explosion venting tank is also connected with the top of the coupling reaction kettle through two pressure type rupture discs, and a needle valve connected with a pressure indicator gauge is arranged between the two pressure type rupture discs.
8. A system for carrying out a coupling reaction according to claim 1, wherein:
a stirring paddle is arranged in the coupling reaction kettle and connected with a motor at the top of the coupling reaction kettle; the coupling reaction kettle is provided with a temperature indicator, a pressure indicator and a liquid level indicator.
9. A system for carrying out a coupling reaction according to claim 1, wherein:
and the exhaust cap is connected with the waste gas pipe after being connected with the butterfly valve.
10. A system for carrying out a coupling reaction according to claim 1, wherein:
and heat insulation layers are arranged on the outer sides of the coupling condenser and the coupling reaction kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921029256.XU CN210449153U (en) | 2019-07-03 | 2019-07-03 | System for realizing coupling reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921029256.XU CN210449153U (en) | 2019-07-03 | 2019-07-03 | System for realizing coupling reaction |
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| Publication Number | Publication Date |
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| CN210449153U true CN210449153U (en) | 2020-05-05 |
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| CN201921029256.XU Active CN210449153U (en) | 2019-07-03 | 2019-07-03 | System for realizing coupling reaction |
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