The invention relates to 4, 4apos; multistage reaction device for continuous production of diaminodiphenyl ether

Abstract

The invention belongs to the technical field of 4, 4 '-diaminodiphenyl ether production devices, and particularly relates to a multi-stage reaction device for continuous production of 4, 4'-diaminodiphenyl ether, which comprises a liquid mixing tank, a multi-stage reaction tank, a second pressure tank, a preheating box, a premixing pipeline, a buffer tank and a first gas supply assembly. 4, 4 '-dinitrodiphenyl ether mixed liquid is preheated through the preheating box, gas-liquid preliminary mixing is firstly performed when the mixed liquid passes through the premixing pipeline, then the mixed liquid is fully mixed through the ultrasonic mixer, a first-stage reaction is performed by utilizing the first catalyst layer, a second-stage reaction is performed in the second catalyst layer through secondary heating, and the mixed liquid is fully mixed through the ultrasonic mixer. According to the process, the reaction efficiency can be greatly improved, the yield is improved, and the production cost of the 4, 4 '-diaminodiphenyl ether can be reduced through the continuous multi-stage reaction production process.

Description

Technical Field

[0001] This invention belongs to the technical field of 4,4'-diaminodiphenyl ether production equipment, specifically a multi-stage reaction device for the continuous production of 4,4'-diaminodiphenyl ether. Background Technology

[0002] 4,4'-Diaminodiphenyl ether (ODA), also known as 4,4'-oxydiphenylamine, is an important organic compound and a crucial chemical intermediate, primarily used in the synthesis of high-performance polymers, such as polyimide (PI)-polyesterimide. These polymers possess excellent heat resistance and mechanical properties, and are widely used in electronics, aerospace, and automotive industries.

[0003] In existing technologies, 4,4'-dinitrodiphenyl ether is commonly used to prepare 4,4'-diaminodiphenyl ether by catalytic hydrogenation. The reaction apparatus (tubular reactor) typically used is a batch reactor, and it can only achieve a first-order reaction, resulting in low reaction efficiency and high production costs. Summary of the Invention

[0004] The purpose of this invention is to provide a multi-stage reaction apparatus for the continuous production of 4,4'-diaminodiphenyl ether, which has the advantages of high reaction efficiency, low production cost, and continuous reaction capability.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0006] A multi-stage reaction apparatus for the continuous production of 4,4'-diaminodiphenyl ether includes a liquid mixing tank, a multi-stage reaction tank, a second pressure tank, a preheating box, a premixing pipeline, a buffer tank, and a first gas supply component. A pump is installed at the outlet of the liquid mixing tank, and the outlet of the pump is connected to the hot water exchange pipe of the preheating box via a pipeline. The outlet of the hot water exchange pipe of the preheating box is connected to the inlet of the premixing pipeline. The outlet of the first gas supply component is connected to the side of the premixing pipeline. The outlet of the premixing pipeline is connected to the buffer tank, and an ultrasonic mixer is installed on the buffer tank. The second pressure tank supplies hydrogen to the multi-stage reaction tank, and the buffer tank supplies a gas-liquid mixture to the multi-stage reaction tank.

[0007] The multi-stage reaction vessel includes:

[0008] The first tank has a reaction product discharge pipe at its bottom and a top cover at its top.

[0009] A uniform dispersion cone disc is arranged in the first tank body and fixedly connected with the top cover, and the uniform dispersion cone disc is connected with the second pressure tank, the edge of the uniform dispersion cone disc extends upward to form a liquid storage area, the liquid storage area is annular, and a gap is arranged on the side of the liquid storage area;

[0010] A first catalyst layer, a transparent guide and a second catalyst layer are sequentially arranged from top to bottom in the first tank body and below the uniform dispersion cone disc, and the second catalyst layer is arranged at the bottom of the first tank body.

[0011] The transparent guide is a shell with an open bottom, and a heating ring is fixedly arranged in the transparent guide.

[0012] Optionally, a plurality of uniformly distributed uniform dispersion pipes are fixedly arranged on the bottom of the uniform dispersion cone disc.

[0013] Optionally, the first catalyst layer comprises a porous tray, a limiting ring is fixedly connected to the inner wall of the first tank body, the porous tray is arranged above the limiting ring, and the catalyst is layered on the porous tray.

[0014] Optionally, the second pressure tank comprises a second tank body, a second pipe is fixedly connected to the top of the second tank body, one end of the second pipe away from the second tank body is fixedly connected with the top cover of the first tank body, and a first flow control valve is arranged on the second pipe.

[0015] Optionally, the preheating box comprises a water tank, a heating element is fixedly arranged in the water tank, the part of the heat exchange water pipe in the water tank is arranged in an “S” shape, and one end of the heat exchange water pipe is connected with the inside of the premixing pipe through a conical sealing element.

[0016] Optionally, the premixing pipe comprises:

[0017] An outer pipe body, one end of the outer pipe body is connected with the buffer tank;

[0018] An inner pipe body, the inner pipe body is arranged in the inner part of the outer pipe body, a spiral sheet is fixedly connected between the outer wall of the inner pipe body and the inner wall of the outer pipe body, and a plurality of micro-holes are arranged on the side of the inner pipe body.

[0019] Optionally, the first gas supply assembly comprises a gas supply pipe, a branch pipe is connected to the side of the gas supply pipe, a second flow control valve is fixedly arranged on the branch pipe, and one end of the branch pipe penetrates through the outer pipe body and is fixedly connected with one end of the inner pipe body.

[0020] Optionally, a mixed liquid injection pipe is fixedly arranged on the top of the liquid mixing tank.

[0021] Compared with the prior art, the beneficial effects of the present application are as follows:

[0022] The application preheats the 4,4'-dinitrodiphenyl ether mixed liquid through a preheating tank, preliminarily mixes gas and liquid through a premixing pipeline, fully mixes through an ultrasonic mixer, and is received through a liquid storage area at the edge of a uniform dispersion cone disc, drops uniformly through a gap into a first catalyst layer full of hydrogen for a first-stage reaction, and then is heated in a second catalyst layer for a second-stage reaction, which can greatly improve the reaction efficiency and the output rate, and the continuous multi-stage reaction production process can reduce the production cost of 4,4'-diaminodiphenyl ether. BRIEF DESCRIPTION OF DRAWINGS

[0023] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or prior art description will be briefly introduced as follows. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor based on these drawings.

[0024] Figure 1 It is a perspective structural schematic diagram of the present application;

[0025] Figure 2 It is a front view structural schematic diagram of the present application;

[0026] Figure 3 It is a top view structural schematic diagram of the present application;

[0027] Figure 4 It is Figure 3 It is a sectional view structural schematic diagram of A-A in the present application;

[0028] Figure 5 It is a perspective structural schematic diagram of the preheating tank and the premixing pipeline of the present application;

[0029] Figure 6 It is Figure 5 It is an enlarged structural schematic diagram of B in the present application.

[0030] In the figure: 1, liquid mixing tank; 1a, mixed liquid injection pipeline; 2, multi-stage reaction tank; 2a, reaction product discharge pipeline; 201, first tank body; 202, uniform distribution cone disc; 202a, uniform distribution pipeline; 203, liquid storage area; 203a, gap opening; 204, first catalyst layer; 204a, porous tray; 204b, catalyst; 205, transparent guide; 206, second catalyst layer; 207, heating ring; 3, second pressure tank; 301, second pipeline; 302, second tank body; 303, first flow control valve; 4, preheating box; 401, water tank; 402, heating element; 403, heat exchange water pipe; 404, conical sealing element; 5, premixing pipeline; 501, outer pipe body; 502, spiral blade; 503, inner pipe body; 503a, micropore; 6, buffer tank; 7, ultrasonic mixer; 8, first gas supply assembly; 801, gas supply pipe; 802, branch pipe; 803, second flow control valve. DETAILED DESCRIPTION

[0031] In order to make the technical problems to be solved by the present application, technical solutions and beneficial effects clearer, the present application will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not to limit the present application.

[0032] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or indirectly connected to the other element.

[0033] It should be understood that the terms "length", "width", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0034] In addition, the terms "first", "second" are only for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the technical features indicated. Therefore, the features defined with "first", "second" can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "multiple" is two or more, unless otherwise specifically limited.

[0035] The present application will now be described with reference to Figures 1-6The multistage reaction device for continuous production of 4,4'-diamino diphenyl ether comprises a liquid mixing tank 1, a multistage reaction tank 2, a second pressure tank 3, a preheating box 4, a premixing pipeline 5, a buffer tank 6 and a first gas supply assembly 8.

[0036] A pump body is installed at the liquid outlet of the liquid mixing tank 1, the liquid outlet end of the pump body is connected with the heat exchange water pipe 403 of the preheating box 4 through a pipeline, the liquid outlet end of the heat exchange water pipe 403 of the preheating box 4 is connected with the feed end of the premixing pipeline 5, the gas outlet end of the first gas supply assembly 8 is connected at the side of the premixing pipeline 5, the discharge end of the premixing pipeline 5 is connected with the buffer tank 6, and an ultrasonic mixer 7 is installed on the buffer tank 6, the second pressure tank 3 supplies hydrogen gas into the multistage reaction tank 2, and the buffer tank 6 supplies liquid mixture into the multistage reaction tank 2.

[0037] The liquid mixing tank 1 stores 4,4'-dinitrodiphenyl ether mixed liquid, which is a mixed liquid of 4,4'-dinitrodiphenyl ether dissolved in a mixed solvent of N,N-dimethylformamide and toluene, the pump body works to pump the mixed liquid in the liquid mixing tank 1 into the heat exchange water pipe 403, the heat exchange water pipe 403 is preheated to 100℃ in the preheating box 4, the water tank 401 generally uses water at 60-90℃, the mixed liquid is preheated by preheating the water at 60-90℃ in the water tank 401 to 100℃, after the mixed liquid is warmed to 100℃, it enters the premixing pipeline 5, at the same time, the gas outlet end of the first gas supply assembly 8 supplies hydrogen gas into the premixing pipeline 5, the hydrogen gas and the mixed liquid are premixed in the premixing pipeline 5 (mixed by flowing in the premixing pipeline 5), then flow into the buffer tank 6, the ultrasonic mixer 7 works to fully mix the mixed liquid mixed with hydrogen gas flowing into the buffer tank 6, and finally the mixed liquid mixed with hydrogen gas flows into the multistage reaction tank 2 for catalytic reaction.

[0038] The multistage reaction tank 2 comprises a first tank body 201, a uniform dispersion cone disc 202, a liquid storage area 203, a first catalyst layer 204, a transparent guide 205, a second catalyst layer 206 and a heating ring 207.

[0039] The bottom of the first tank body 201 is provided with a reaction product discharge pipeline 2a, and the top of the first tank body 201 has a top cover, so that the inside of the first tank body 201 forms a sealed structure, the uniform dispersion cone disc 202 is located in the first tank body 201, and the uniform dispersion cone disc 202 is fixedly connected with the top cover, the uniform dispersion cone disc 202 is connected with the second pressure tank 3, hydrogen gas with a certain pressure is introduced into the inside of the second pressure tank 3 through an external hydrogen tank, the pressure is controlled to be 1 MPa, the edge of the uniform dispersion cone disc 202 extends upwards to form a liquid storage area 203, the liquid storage area 203 is annular, gap openings 203a are formed in the side surface of the liquid storage area 203, and the inside of the first tank body 201 and below the uniform dispersion cone disc 202 are sequentially provided with a first catalyst layer 204, a transparent guide 205 and a second catalyst layer 206 from top to bottom, the second catalyst layer 206 is located at the bottom of the first tank body 201, the transparent guide 205 is a shell with an open bottom, the transparent guide 205 is made of borosilicate glass, and a heating ring 207 is fixedly installed in the inside of the transparent guide 205.

[0040] The catalytic process in the multi-stage reaction tank 2 is as follows: the second pressure tank 3 continuously transports hydrogen gas into the inside of the first tank body 201, so that the mixed liquid in the buffer tank 6 flows into the first tank body 201, falls into the annular liquid storage area 203 and uniformly drops downwards along the gap openings 203a formed in the side surface of the liquid storage area 203, the mixed liquid enters the first catalyst layer 204 to perform a first-stage catalytic reaction, then the liquid penetrates downwards through the first catalyst layer 204, the heating ring 207 installed in the inside of the transparent guide 205 performs secondary heating on the bottom layer of the first catalyst layer 204, and the liquid falls into the second catalyst layer 206 to perform a second-stage catalytic reaction; the shell of the transparent guide 205 plays a guiding role.

[0041] Compared with the prior art, the multi-stage reaction device for continuous production of 4,4'-diamino diphenyl ether provided by the application adopts a preheating box 4 to preheat 4,4'-dinitrodiphenyl ether mixed liquid, the mixed liquid is preliminarily mixed with gas through a premixing pipeline 5, then is fully mixed through an ultrasonic mixer 7, is received through the liquid storage area 203 at the edge of the uniform dispersion cone disc 202, uniformly drops into the first catalyst layer 204 full of hydrogen gas to perform a first-stage reaction, and then is heated in the second catalyst layer 206 to perform a second-stage reaction, so that the reaction efficiency of the 4,4'-dinitrodiphenyl ether mixed liquid can be greatly improved, the yield is improved, and the production cost of 4,4'-diamino diphenyl ether can be reduced through the continuous multi-stage reaction production process.

[0042] In another embodiment of the application, please refer to Figure 4The bottom of the uniform dispersion cone disc 202 is fixedly connected with a plurality of uniformly distributed uniform dispersion pipes 202a, a plurality of air holes are arranged in the uniform dispersion pipe 202a, the air holes pass through the whole uniform dispersion pipe 202a, a conical cavity is arranged in the inside of the uniform dispersion cone disc 202, the air holes are communicated with the conical cavity, the top of the plurality of uniformly distributed uniform dispersion pipes 202a is communicated with the inside of the conical cavity, and the bottom of the plurality of uniformly distributed uniform dispersion pipes 202a is directed downwards (towards the first catalyst layer 204), which is helpful for hydrogen to enter through the top of the uniform dispersion pipe 202a and be sprayed out through the bottom, thereby being sprayed into the first catalyst layer 204.

[0043] In another embodiment of the present application, referring to Figure 4 The first catalyst layer 204 comprises a porous tray 204a, and a catalyst 204b is arranged in the porous tray 204a; the inner wall of the first tank body 201 is fixedly connected with a limiting ring, and the porous tray 204a is arranged above the limiting ring; and the catalyst 204b is arranged in a layer on the porous tray 204a.

[0044] In another embodiment of the present application, referring to Figure 4 The second pressure tank 3 comprises a second tank body 302, and a second pipe 301 is fixedly connected to the top of the second tank body 302; one end of the second pipe 301, which is away from the second tank body 302, is fixedly connected with the top cover of the first tank body 201; and a first flow control valve 303 is arranged on the second pipe 301.

[0045] Hydrogen with a certain pressure is introduced into the second pressure tank 3 through an external hydrogen tank, and the pressure is controlled to be 1 MPa; and the flow rate of the hydrogen sprayed out through the second pipe 301 can be adjusted by controlling the first flow control valve 303.

[0046] In another embodiment of the present application, referring to Figures 1 to 5 The preheating box 4 comprises a water tank 401, and a heating element 402 is fixedly arranged in the inside of the water tank 401; the part of a heat exchange water pipe 403 in the inside of the water tank 401 is arranged in an “S” shape; and one end of the heat exchange water pipe 403 is connected with the inside of the premixing pipe 5 through a conical sealing element 404.

[0047] The heating element 402 is an electric heating copper pipe, directly heats the water in the inside of the water tank 401, and the part of the heat exchange water pipe 403 in the inside of the water tank 401 is arranged in an “S” shape, so that the heat exchange area is increased and the heat exchange efficiency is improved.

[0048] In another embodiment of the present application, referring to Figure 5 and Figure 6The premixing pipeline 5 comprises an outer pipe body 501 and an inner pipe body 503, one end of the outer pipe body 501 is connected with the buffer tank 6, the inner pipe body 503 is arranged in the inner part of the outer pipe body 501, the helical blade 502 is fixedly connected between the outer wall of the inner pipe body 503 and the inner wall of the outer pipe body 501, a plurality of micropores 503a are arranged on the side surface of the inner pipe body 503, and the pore size of the micropores 503a is 0.5 nanometers.

[0049] The hydrogen is discharged from the micropores 503a through the inner pipe body 503, since the hydrogen molecules contained in the hydrogen have a diameter of about 0.289 nanometers, the micropores 503a with the pore size of 0.5 nanometers are arranged, so that the hydrogen can be uniformly and stably introduced into the inner part of the outer pipe body 501, the mixed liquid is guided to flow spirally by the helical blade 502, the mixed liquid in spiral flow is fully contacted with the hydrogen, and the hydrogen is partially dissolved in the mixed liquid.

[0050] In another embodiment of the present application, referring to Figure 5 and Figure 6 The first gas supply assembly 8 comprises a gas supply pipe 801, the side surface of the gas supply pipe 801 is connected with a branch pipe 802, the second flow control valve 803 is fixedly installed on the branch pipe 802, and one end of the branch pipe 802 penetrates through the outer pipe body 501 and is fixedly connected with one end of the inner pipe body 503.

[0051] The hydrogen with a certain pressure is introduced into the gas supply pipe 801 through the external hydrogen tank, the pressure is controlled to be 1 MPa, the hydrogen is introduced into the inner pipe body 503 through the gas supply pipe 801 and the branch pipe 802, and then is sprayed out from the micropores 503a on the side surface of the inner pipe body 503, and the flow rate of the hydrogen is controlled by the second flow control valve 803.

[0052] In another embodiment of the present application, referring to Figure 1 The top of the liquid mixing tank 1 is fixedly provided with a mixed liquid injection pipeline 1a, and the mixed liquid can be added into the liquid mixing tank 1 through the mixed liquid injection pipeline 1a.

[0053] The above only describes the preferred embodiments of the present application and should not be used to limit the present application, and any modification, equivalent replacement and improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A multi-stage reaction apparatus for the continuous production of 4,4'-diaminodiphenyl ether, characterized in that, The system includes a liquid mixing tank (1), a multi-stage reaction tank (2), a second pressure tank (3), a preheating box (4), a premixed pipeline (5), a buffer tank (6), and a first gas supply assembly (8). The liquid mixing tank (1) is equipped with a pump body at its outlet. The outlet of the pump body is connected to the heat exchange pipe (403) of the preheating box (4) via a pipeline. The outlet of the heat exchange pipe (403) of the preheating box (4) is connected to the feed end of the premixed pipeline (5). The gas outlet of the first gas supply assembly (8) is connected to the side of the premixed pipeline (5). The discharge end of the premixed pipeline (5) is connected to the buffer tank (6). An ultrasonic mixer (7) is installed on the buffer tank (6). The second pressure tank (3) supplies hydrogen to the multi-stage reaction tank (2). The buffer tank (6) supplies gas-liquid mixture to the multi-stage reaction tank (2). The multi-stage reaction vessel (2) includes: The first tank (201) has a reaction product discharge pipe (2a) at its bottom and a top cover at its top. A uniform dispersion cone (202) is located inside the first tank (201) and is fixedly connected to the top cover. The uniform dispersion cone (202) is connected to the second pressure tank (3). The edge of the uniform dispersion cone (202) extends upward to form a liquid storage area (203). The liquid storage area (203) is annular and has a gap opening (203a) on its side. Inside the first tank (201) and below the uniform distribution cone (202), a first catalyst layer (204), a transparent guide (205), and a second catalyst layer (206) are arranged sequentially from top to bottom, with the second catalyst layer (206) located at the bottom of the first tank (201). The transparent guide (205) is a shell with an opening at the bottom, and a heating ring (207) is fixedly installed inside the transparent guide (205).

2. The multi-stage reaction apparatus for continuous production of 4,4'-diaminodiphenyl ether as described in claim 1, characterized in that: Multiple uniformly distributed distribution pipes (202a) are fixedly installed on the bottom fixed sealing plate of the distribution cone (202).

3. The multi-stage reaction apparatus for continuous production of 4,4'-diaminodiphenyl ether as described in claim 1, characterized in that: The first catalyst layer (204) includes a porous tray (204a), and a limiting ring is fixedly connected to the inner wall of the first tank (201). The porous tray (204a) is disposed above the limiting ring, and the catalyst (204b) is spread in layers on the porous tray (204a).

4. The multi-stage reaction apparatus for continuous production of 4,4'-diaminodiphenyl ether as described in claim 1, characterized in that, The second pressure tank (3) includes a second tank body (302), a second pipe (301) is fixedly connected to the top of the second tank body (302), and the end of the second pipe (301) away from the second tank body (302) is fixedly connected to the top cover of the first tank body (201). A first flow control valve (303) is installed on the second pipe (301).

5. The multi-stage reaction apparatus for continuous production of 4,4'-diaminodiphenyl ether as described in claim 1, characterized in that: The preheating box (4) includes a water tank (401), and a heating element (402) is fixedly installed inside the water tank (401). The portion of the hot water exchange pipe (403) inside the water tank (401) is distributed in an "S" shape. One end of the hot water exchange pipe (403) is connected to the inside of the premixed pipe (5) through a conical seal (404).

6. The multi-stage reaction apparatus for the continuous production of 4,4'-diaminodiphenyl ether as described in claim 1, characterized in that, The premixed pipeline (5) includes: An outer tube (501) is connected at one end to a buffer tank (6); An inner tube (503) is disposed inside an outer tube (501). A spiral blade (502) is fixedly connected between the outer wall of the inner tube (503) and the inner wall of the outer tube (501). Several micro-holes (503a) are opened on the side of the inner tube (503).

7. The multi-stage reaction apparatus for continuous production of 4,4'-diaminodiphenyl ether as described in claim 6, characterized in that, The first gas supply assembly (8) includes a gas supply pipe (801), a branch pipe (802) is connected to the side of the gas supply pipe (801), a second flow control valve (803) is fixedly installed on the branch pipe (802), one end of the branch pipe (802) passes through the outer pipe body (501) and is fixedly connected to one end of the inner pipe body (503).

8. The multi-stage reaction apparatus for continuous production of 4,4'-diaminodiphenyl ether as described in claim 1, characterized in that: The top of the liquid mixing tank (1) is fixedly provided with a liquid injection pipe (1a).

Images