Preparation of acidic glyphosate mother liquor recovery distillation device of triethylamine

By combining the design of spiral heating tubes, defoaming structure and flow splitting structure, the problems of uneven solution heating and insufficient heat dissipation of heat transfer oil were solved, the distillation efficiency of acidic glyphosate mother liquor was improved, and triethylamine was recovered efficiently.

CN117258340BActive Publication Date: 2026-02-06ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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Patent Information

Application Number
CN202311328172.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-10-13
Publication Date
2026-02-06
Estimated Expiration
2043-10-13

AI Technical Summary

Technical Problem

Existing distillation kettles suffer from uneven heating of the solution and insufficient heat transfer oil during the heating process, resulting in low distillation efficiency.

Method used

It adopts a combination design of spiral heating tube heating structure, defoaming structure and flow-dividing structure. The spiral heating tube provides all-round heating, the motor-driven foam eliminator removes bubbles, and the flow-dividing structure changes the rotation direction to achieve uniform stirring and heating of the solution.

Benefits of technology

This method achieves uniform heating and sufficient heat dissipation of the solution, improves distillation efficiency, and enhances the recovery efficiency of triethylamine.

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Abstract

The application discloses an acid glyphosate mother liquor preparation triethylamine recovery rectification device, which comprises a tank body, the surface of the tank body is provided with an inlet, the inside of the tank body is provided with a heating structure, the spiral heating pipe of the heating structure is arranged in the inner cavity of the tank body, the top is provided with a defoaming structure, the mounting plate of the defoaming structure is arranged on the inner cavity wall of the tank body, the lower portion of the mounting plate is rotatably provided with a connecting disc, the outer ring of the connecting disc is provided with a foam catching net, and the lower portion of the defoaming structure is provided with a shunt structure.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of glyphosate production, and particularly to a three-ethylamine recovery rectification device prepared from an acid glyphosate mother liquor. BACKGROUND

[0002] Three-ethylamine is a catalyst in the production process of glyphosate, and the product yield is closely related to the three-ethylamine content and water content. The production of glyphosate by alkyl esterification method will produce a large amount of acid glyphosate mother liquor, which needs to be rectified to extract and recover three-ethylamine, so as to reduce the production cost of acid glyphosate mother liquor.

[0003] Generally, the acid glyphosate mother liquor is rectified in a rectification kettle to recover and utilize three-ethylamine. For example, a rectification kettle disclosed in CN218653039U includes a rectification kettle main body, the rectification kettle main body includes a kettle body, a drain pipe is fixedly connected to the center of the bottom of the kettle body, a kettle cover is connected and installed on the top of the kettle body through a connecting flange, a steam outlet is formed in the top of the kettle cover, and a feed inlet is formed in one side of the kettle body.

[0004] However, this rectification kettle only heats and rectifies the internal solution through the internal spiral heat conducting oil pipe, and the materials statically placed in the kettle body cannot be fully heated during the rectification process, which limits the rectification efficiency. Meanwhile, the upward and downward heat conducting oil pipes make the hot oil flow too fast in the internal pipe and cannot be fully dispersed. SUMMARY

[0005] The present application aims to solve the problems of the background technology that the solution statically placed in the kettle body is not uniformly heated and rectified, which limits the rectification efficiency, and the upward and downward heat conducting oil pipes cannot fully disperse the heat in the pipe, and proposes a three-ethylamine recovery rectification device prepared from an acid glyphosate mother liquor.

[0006] The purpose of the present application can be achieved by the following technical solutions:

[0007] The three-ethylamine recovery rectification device prepared from an acid glyphosate mother liquor includes a kettle body, a feed inlet is formed on the surface of the kettle body, a heating structure is arranged in the internal cavity of the kettle body, a spiral heating pipe of the heating structure is arranged in the internal cavity of the kettle body, an oil inlet and an oil outlet are arranged at both ends of the spiral heating pipe, the oil inlet and the oil outlet extend out of the internal cavity of the kettle body to the outside of the kettle body;

[0008] A defoaming structure is arranged on the top of the kettle body, a mounting plate of the defoaming structure is arranged on the inner cavity wall of the kettle body, a connecting disc is rotatably arranged below the mounting plate, a foam catching net is arranged on the outer circle of the connecting disc, and the foam catching net is in contact with the bottom surface of the mounting plate;

[0009] A flow dividing structure is arranged below the defoaming structure, and the flow dividing structure includes:

[0010] The connecting column is arranged in the middle of the spiral heating pipe, and the surface of the connecting column is provided with a plurality of flow distribution plates, each of which is rotatably connected with the surface of the connecting column.

[0011] A plurality of flow channels are arranged on both sides of each flow distribution plate, and the aperture of each flow channel decreases from large to small along the same rotation direction.

[0012] A blocking ball is elastically connected with the side of the flow channel with a smaller aperture, and the flow channel is provided with a flow passage which can be directly contacted with the blocking ball, and the radius of the flow passage is smaller than that of the blocking ball.

[0013] As a further scheme of the present application, the top of the mounting plate is provided with a motor, the output end of the motor is arranged through the mounting plate, and the output end of the motor is coaxially fixedly connected with the connecting disc, and the outer surface of the motor is provided with a protective shell.

[0014] As a further scheme of the present application, a plurality of flow distribution plates are arranged at equal intervals on the circumferential surface of the connecting column, and the flow distribution plates of different layers are arranged in a staggered manner.

[0015] As a further scheme of the present application, the top of the flow distribution plate is provided with two connecting blocks, and a rotating shaft is fixedly arranged between the two connecting blocks and rotatably connected with the surface of the connecting column.

[0016] As a further scheme of the present application, the side of the flow channel with a smaller aperture is provided with a mounting ring, the inner side of the mounting ring is provided with a reset spring, and the reset spring is fixedly connected with the surface of the blocking ball.

[0017] As a further scheme of the present application, the oil inlet is arranged below the oil outlet.

[0018] As a further scheme of the present application, the top of the tank body is provided with a mounting cover, and the tank body and the mounting cover are detachably fixedly connected through fixing bolts.

[0019] As a further scheme of the present application, the top of the mounting cover is provided with an air outlet, and the bottom of the tank body is provided with a discharge port.

[0020] As a further scheme of the present application, the bottom of the tank body is provided with a plurality of support frames arranged at equal intervals in the circumferential direction.

[0021] As a further scheme of the present application, the outer ring of the foam catching net is provided with a connecting ring, and the shape of the connecting ring is adapted to the inner cavity of the tank body.

[0022] The present application has the following advantages:

[0023] (1) The acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application, by setting up the heating structure, the heating structure is provided with a spiral heating pipe in the inner cavity of the tank, the solution of the tank is heated and warmed in all directions, the oil inlet is arranged below the oil outlet, so that the hot oil can slowly move in the spiral heating pipe and be fully heated;

[0024] (2) The acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application, by setting up the defoaming structure, the motor of the defoaming structure can drive the relative rotation between the foam catcher and the mounting plate, so that the foam attached to the foam catcher is eliminated by the mounting plate;

[0025] (3) The acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application, by setting up the shunt structure, the connecting column of the shunt structure will rotate with the connecting disc, when the connecting column rotates, the rotation direction makes the solution flow from the side with smaller aperture to the side with larger aperture, at this time, the blocking ball will be affected by the force of the liquid pressure and the return spring, and the flow passage will be blocked, so that the solution cannot pass through the flow passage, and the shunt plate only plays the role of uniform stirring of the solution and work heating; when the connecting column rotates reversely, the combined force of the liquid pressure and the return spring acting on the blocking ball makes the blocking ball separate from the flow passage, and the solution is shunted from the flow passage;

[0026] (4) The acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application, by setting up the shunt structure inside the heating structure, the shunt structure is driven to rotate the internal solution while the defoaming structure is defoaming, the solution is worked to improve the temperature or the liquid is guided to contact the spiral heating pipe of the heating structure through the shunt, so as to increase the contact area of the internal flowing solution with the heating structure, thereby improving the rectification efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0027] The present application will be further described below in conjunction with the drawings.

[0028] Figure 1 is the structure diagram of the acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application;

[0029] Figure 2 is the front view of the acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application;

[0030] Figure 3 is the front view of the acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application;

[0031] Figure 4 is the front view of the acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application;

[0032] Figure 5is a structural schematic diagram of the bubble removing structure of the present application;

[0033] Figure 6 is a bottom view schematic diagram of the bubble removing structure of the present application;

[0034] Figure 7 is a structural schematic diagram of the flow dividing structure of the present application;

[0035] Figure 8 is a sectional view schematic diagram of the flow dividing plate of the present application;

[0036] Figure 9 is a local enlarged view of the flow dividing plate of the present application.

[0037] In the figure: 1, tank body; 2, mounting cover; 21, fixing bolt; 3, feeding port; 4, heating structure; 41, oil inlet; 42, spiral heating pipe; 43, oil outlet; 5, bubble removing structure; 51, mounting plate; 52, protective shell; 53, motor; 54, connecting disc; 55, foam catching net; 56, connecting ring; 6, flow dividing structure; 61, connecting column; 62, flow dividing plate; 63, connecting block; 64, rotating shaft; 65, flow channel; 66, mounting ring; 67, reset spring; 68, blocking ball; 69, flow passage; 7, support frame; 8, air outlet; 9, discharge port. DETAILED DESCRIPTION

[0038] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present application.

[0039] Please refer to Figures 1-9 The present application is an acid glyphosate mother liquor preparation triethylamine recovery rectification device, which comprises a tank body 1. A mounting cover 2 is detachably arranged on the top of the tank body 1, and the tank body 1 and the mounting cover 2 are detachably fixedly connected through a plurality of fixing bolts 21. A feeding port 3 is arranged on one side of the tank body 1, and the feeding port 3 is in communication with the inner cavity of the tank body 1. A plurality of circumferentially arranged support frames 7 are arranged on the outer surface of the bottom of the tank body 1. A discharge port 9 is arranged at the bottom of the tank body 1, and the discharge port 9 is in communication with the inner cavity of the tank body 1. A heating structure 4 is arranged in the inner cavity of the tank body 1. An oil inlet 41 of the heating structure 4 extends into the inner cavity of the tank body 1 from the outside of the tank body 1. A spiral heating pipe 42 is in communication with the end of the oil inlet 41 extending into the inner cavity. The spiral heating pipe 42 is arranged in the inner cavity of the tank body 1 in a spiral ascending manner. An oil outlet 43 is in communication with the end of the spiral heating pipe 42 away from the oil inlet 41. The oil outlet 43 extends out of the inner cavity of the tank body 1 to the outer surface of the tank body 1, and the oil outlet 43 is located above the oil inlet 41.

[0040] The inside of the tank body 1 is provided with a defoaming structure 5, the mounting plate 51 of the defoaming structure 5 is arranged in the inner cavity of the tank body 1, both ends of the mounting plate 51 are fixedly connected with the inner cavity wall of the tank body 1, the top of the mounting plate 51 is provided with a protective shell 52, the inside of the protective shell 52 is provided with a motor 53, the output end of the motor 53 is arranged vertically downward, the output end of the motor 53 extends to the lower side of the mounting plate 51 through the mounting plate 51. The output end of the motor 53 is fixedly provided with a connecting disc 54, the both sides of the connecting disc 54 are provided with a foam catching net 55, the outer ring of the foam catching net 55 is fixedly provided with a connecting ring 56, the connecting ring 56 is adapted to the shape of the inner cavity of the tank body 1.

[0041] The lower side of the defoaming structure 5 is provided with a shunt structure 6, the connecting column 61 of the shunt structure 6 is fixedly arranged at the bottom of the connecting disc 54, the connecting column 61 is arranged in the inside of the spiral heating pipe 42; the connecting column 61 and the center axis of the connecting disc 54 are located on the same vertical line. The circumferential surface of the connecting column 61 is provided with a plurality of shunt plates 62, a plurality of shunt plates 62 are arranged on the circumferential surface of the connecting column 61 at equal intervals, and the shunt plates 62 at different vertical positions are arranged staggered. The top of each shunt plate 62 is provided with a connecting block 63, the connecting blocks 63 are fixedly provided with a rotating shaft 64, the rotating shaft 64 penetrates the surface of the connecting column 61, so that the rotating shaft 64 is rotatably connected with the connecting column 61, and the shunt plate 62 is rotatable relative to the connecting column 61. The inside of the shunt plate 62 is provided with a plurality of flow channels 65, the plurality of flow channels 65 penetrate the both sides of the shunt plate 62, and the flow channels 65 on the same rotating direction of the connecting column 61 change from large to small along the same radius of the connecting column 61. The side with smaller aperture of each flow channel 65 is provided with a mounting ring 66, the inner side of the mounting ring 66 is fixedly provided with a reset spring 67, the side away from the mounting ring 66 of the reset spring 67 is fixedly provided with a plug ball 68, the inside of the flow channel 65 is provided with a flow port 69, the flow port 69 can be in contact with the plug ball 68, and the radius of the flow port 69 is smaller than the radius of the plug ball 68.

[0042] When using this acidic glyphosate mother liquor to prepare a triethylamine recovery rectification device, the glyphosate acidic mother liquor is stored in the inner cavity of the tank body 1 along with the catalyst triethylamine through the inlet 3. Then the material inside the tank body 1 is heated and rectified by the heating structure 4, the high-temperature heat transfer oil is injected from the oil inlet 41, finally discharged from the oil outlet 43 to form a heat oil circulation through the spiral heating pipe 42 inside. Thus the temperature of the inner cavity of the tank body 1 is raised to achieve the effect of rectifying triethylamine. When the glyphosate solution is heated and converted into gas, it is discharged from the inside of the tank body 1 through the upper gas outlet 8. The gas bubbles generated during the movement of the gas in the solution will adhere to the foam trap 55, and the gas will separate from the bubbles after passing through the foam trap 55 and be discharged upward. At this time, the motor 53 is started, and the output end of the motor 53 drives the connecting disc 54 to rotate, and the foam traps 55 on both sides of the connecting disc 54 will continuously rotate relative to the fixedly arranged mounting plate 51 during rotation, so that the mounting plate 51 eliminates the bubbles on the surface of the foam trap 55. While the defoaming structure 5 is working, the rotation of the connecting disc 54 will drive the lower flow dividing structure 6 to divide. The connecting column 61 is driven by the connecting disc 54 to rotate in one direction, and the several flow dividing plates 62 arranged on the surface of the connecting column 61 will be subjected to centrifugal force and will rotate away from the connecting column 61, so that the connecting column 61 can increase the range of its contact with the solution. The rotating direction of the connecting column 61 makes the solution flow from the side with smaller aperture to the side with larger aperture of the flow channel 65, at this time the blocking ball 68 will be subjected to the force of the liquid and the pressure of the return spring 67, so that the blocking ball 68 tightly contacts the flow-through opening 69, so that the liquid cannot pass through the flow-through channel 65. In turn, the flow dividing plate 62 can only play a role in stirring the solution, which further raises the temperature of the inner cavity of the tank body 1 while fully heating the solution. Then the motor 53 drives the connecting column 61 to rotate in the opposite direction, at this time the solution flows from the side with larger aperture to the side with smaller aperture of the flow-through channel 65, at this time the blocking ball 68 is subjected to the combined force of the liquid pressure and the elastic force of the return spring 67, so that the blocking ball 68 can move away from the flow-through opening 69, so that the solution can pass through the flow-through channel 65. The liquid discharged from the flow-through channel 65 during the rotation of the flow dividing plate 62 will be thrown out and directly contact the spiral heating pipe 42 on the outside, thereby increasing the contact surface between the liquid and the spiral heating pipe 42 and increasing the rectification efficiency of the rectification device.

[0043] The working principle of the present application: the acid glyphosate mother liquor preparation triethylamine recovery rectification device of the present application is provided with a heating structure 4, the heating structure 4 is provided with a spiral heating pipe 42 in the inner cavity of the tank body 1, the solution in the tank body 1 is heated and warmed in all directions, the oil inlet 41 is arranged below the oil outlet 43, so that the hot oil can slowly move in the spiral heating pipe 42 and be fully heated; the defoaming structure 5 is provided, the motor 53 of the defoaming structure 5 can drive the relative rotation between the foam catching net 55 and the mounting plate 51, so that the foam attached to the foam catching net 55 is eliminated by the mounting plate 51; the shunt structure 6 is provided, the connecting column 61 of the shunt structure 6 will rotate with the connecting disc 54, when the connecting column 61 rotates, the rotation direction makes the solution flow from the side with smaller aperture to the side with larger aperture of the flow channel 65, at this time, the blocking ball 68 will be affected by the liquid pressure and the force of the return spring 67, and the flow-through opening 69 is blocked, so that the solution cannot pass through the flow channel 65, the shunt plate 62 only plays the role of uniform stirring of the solution and work heating; when the connecting column 61 rotates reversely, the combined force of the liquid pressure and the force of the return spring 67 acting on the blocking ball 68 makes the blocking ball 68 separate from the flow-through opening 69, the solution in the flow channel 65 is shunted, and directly contacts the spiral heating pipe 42 outside when being discharged, the defoaming operation of the defoaming structure 5 is carried out at the same time, the shunt structure 6 is driven to rotate the internal solution, the solution is worked to improve the temperature or the liquid is guided to contact the spiral heating pipe 42 of the heating structure 4, so that the contact area of the internal flowing solution with the heating structure 4 is increased, thereby improving the rectification efficiency.

[0044] The above has carried out the detailed description to one embodiment of the present application, but the content described is only the preferred embodiment of the present application, and cannot be considered as being used for limiting the implementation scope of the present application. Any equivalent change and improvement made according to the application scope of the present application should still belong to the patent coverage scope of the present application.

Claims

1. The triethylamine recovery rectification device for preparing acidic glyphosate mother liquor comprises a tank body (1), and a feeding port (3) is arranged on the surface of the tank body (1), characterized in that, The inside of the tank body (1) is provided with a heating structure (4), the spiral heating pipe (42) of the heating structure (4) is arranged in the inner cavity of the tank body (1), and the two ends of the spiral heating pipe (42) are respectively provided with an oil inlet (41) and an oil outlet (43); the oil inlet (41) and the oil outlet (43) extend from the inner cavity of the tank body (1) to the outside of the tank body (1); The top of the tank body (1) is provided with a defoaming structure (5), the mounting plate (51) of the defoaming structure (5) is arranged on the inner cavity wall of the tank body (1), the lower side of the mounting plate (51) is rotatably provided with a connecting disc (54), the outer ring of the connecting disc (54) is provided with a foam catching net (55), and the foam catching net (55) is in contact with the bottom surface of the mounting plate (51); The lower side of the defoaming structure (5) is provided with a shunt structure (6), and the shunt structure (6) comprises: A connecting column (61) is arranged at the bottom of the connecting disc (54), the connecting column (61) is arranged in the middle of the spiral heating pipe (42), and the surface of the connecting column (61) is provided with a plurality of shunt plates (62); each shunt plate (62) is rotatably connected with the surface of the connecting column (61); A plurality of flow channels (65) are arranged on both sides of each shunt plate (62), and each flow channel (65) decreases in aperture along the same rotation direction from large to small; A blocking ball (68) is elastically connected with the side with smaller aperture of the flow channel (65), the flow channel (65) is provided with a flow passage (69), the flow passage (69) can be in direct contact with the blocking ball (68), and the radius of the flow passage (69) is smaller than that of the blocking ball (68).

2. The apparatus for preparing triethylamine recovery distillation from the acidic glyphosate mother liquor according to claim 1, characterized in that, The top of the mounting plate (51) is provided with a motor (53), the output end of the motor (53) penetrates the mounting plate (51), the output end of the motor (53) is fixedly connected with the connecting disc (54) in a coaxial manner, and the outer surface of the motor (53) is provided with a protective shell (52).

3. The apparatus for preparing triethylamine recovery rectification of acid glyphosate mother liquor according to claim 1, characterized in that, The plurality of shunt plates (62) are circumferentially arranged at equal distances and arranged on the circumferential surface of the connecting column (61), and the shunt plates (62) of different layers are arranged alternately.

4. The apparatus for preparing triethylamine recovery rectification of acid glyphosate mother liquor according to claim 1, characterized in that, The top of the shunt plate (62) is provided with two connecting blocks (63), the two connecting blocks (63) are fixedly provided with a rotating shaft (64), and the rotating shaft (64) penetrates the surface of the connecting column (61) and is rotatably connected therewith.

5. The apparatus for preparing triethylamine recovery rectification of acid glyphosate mother liquor according to claim 1, characterized in that, The side with smaller aperture of the flow channel (65) is provided with a mounting ring (66), the inner side of the mounting ring (66) is provided with a reset spring (67), and the reset spring (67) is fixedly connected with the surface of the blocking ball (68).

6. The apparatus for preparing triethylamine recovery rectification of acid glyphosate mother liquor according to claim 1, characterized in that, The oil inlet (41) is arranged below the oil outlet (43).

7. The apparatus for preparing triethylamine recovery rectification of acid glyphosate mother liquor according to claim 1, characterized in that, The top of the tank body (1) is provided with a mounting cover (2), and the tank body (1) and the mounting cover (2) are detachably fixedly connected through fixing bolts (21).

8. The apparatus for preparing triethylamine recovery distillation from the acidic glyphosate mother liquor according to claim 7, characterized in that, The top of the mounting cover (2) is provided with an air outlet (8), and the bottom of the tank body (1) is provided with a discharge port (9).

9. The apparatus for preparing triethylamine recovery rectification of acid glyphosate mother liquor according to claim 1, characterized in that, The bottom of the tank body (1) is provided with a plurality of support frames (7) arranged at equal distances and in a circumferential array.

10. The apparatus for recovering triethylamine from the preparation of an acidic glyphosate mother liquor according to claim 1, characterized in that The outer ring of the foam catching net (55) is provided with a connecting ring (56), and the shape of the connecting ring (56) is adapted to the inner cavity of the tank body (1).

Citation Information

Patent Citations

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