A device for treating dimetholine synthesis reaction evaporation product

By designing the extraction tower and salt washing tower system for evaporation treatment of enoylmorpholine synthesis reaction, combined with the automatic control system, the problems of discontinuity, low efficiency and poor accuracy in the prior art are solved, automatic continuous production and efficient dehydration are achieved, and production efficiency and product quality are improved.

CN222723660UActive Publication Date: 2025-04-08LIAONING CYNDA CHEM CO LTD
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Patent Information

Application Number
CN202421453087.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-06-24
Publication Date
2025-04-08
Estimated Expiration
2034-06-24

AI Technical Summary

Technical Problem

The existing evaporation treatment process for synthesis of enoylmorpholine has discontinuous production, low efficiency, large energy consumption, and manual operation of process control, resulting in poor accuracy and affecting production efficiency and product quality.

Method used

A treatment device for the evaporation of enoylmorpholine synthesis reaction is designed, including an extraction tower, a salt washing tower and an automatic control system. By automatically controlling the material feed quantity and feed rate of the extraction tower, the proportional mixing and dehydration of water and tert-butanol xylene is achieved, thereby reducing manual operation.

Benefits of technology

Automatic continuous production is achieved, production efficiency is improved, labor intensity and energy consumption are reduced, and product quality is improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model belongs to the technical field of chemical production, and discloses a processing device for the distillate of the ethylene methacrylate synthesis reaction, comprising an extraction tower, wherein the upper part of the extraction tower is respectively connected with a washing water pipeline and a water-containing xylene output pipeline, the washing water pipeline is provided with a water flow meter and a water regulating valve, the water-containing xylene output pipeline is connected to the water-containing xylene receiving tank; the bottom of the water-containing xylene receiving tank is connected to the lower feed port of the salt washing tower through a pipeline, a valve and a feed pump, the upper part of the salt washing tower is connected with an anhydrous xylene discharge pipeline, the anhydrous xylene discharge pipeline is connected to the anhydrous xylene receiving tank; the lower part of the extraction tower is connected with a tert-butyl alcohol xylene feed pipeline, the tert-butyl alcohol xylene feed pipeline is provided with a distillate flow meter and a distillate regulating valve; the bottom of the extraction tower is connected with a water phase discharge pipe, the water phase discharge pipe is connected to the water phase receiving tank. The utility model can improve production efficiency, realize automatic continuous production, reduce labor intensity; and can reduce energy consumption and reduce costs.
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Description

Technical Field

[0001] The utility model belongs to the technical field of chemical production, and in particular relates to a device for processing dimetholine synthesis reaction distillates. Background Art

[0002] Dimethomorph is a broad-spectrum fungicide of the morpholine class. It is a specific agent for the prevention and control of Oomycete fungal diseases. It has a good preventive and control effect on low-level fungal diseases such as downy mildew, downy mildew, late blight, blight, blight rot, pythium, and black shank.

[0003] The synthesis of oxadiazine is carried out by using sodium tert-butoxide as a condensation catalyst and xylene as a solvent to synthesize acetylmorpholine and 3,4-dimethoxy-4-chloro-benzophenone. During the synthesis process, the by-product tert-butanol needs to be distilled out to ensure that the reaction continues in the target direction and achieve the expected yield of the reaction. Because xylene will be distilled out together with tert-butanol in an azeotropic manner, the distillation product is a xylene solution containing tert-butanol. If the xylene needs to be recovered and reused, the tert-butanol needs to be washed away with water first, and then the xylene needs to be dehydrated to make the water content ≤0.1% before it can be used.

[0004] The prior art is to add xylene containing tert-butyl alcohol and water into a layering kettle, stir for 30 minutes, and then let it stand for 30 minutes to layer. The upper layer is xylene containing about 1% water, and the lower layer is a tert-butyl alcohol aqueous solution (tert-butyl alcohol is dissolved in water and discharged with water); the xylene containing tert-butyl alcohol is washed with water three times, and then the xylene is transferred to a distillation tower for distillation reflux dehydration. When the water content is ≤0.1%, the temperature is lowered to 30°C and poured into an anhydrous xylene storage tank for application. It can be seen that the prior art has the following defects: discontinuous production, low production efficiency, and large energy consumption; and the process control requires manual operation, poor accuracy, and seriously affects production efficiency and product quality. Summary of the invention

[0005] The technical problem to be solved by the utility model is to provide a device for processing distilled product of enoylmorpholine synthesis reaction, which overcomes the defects of the prior art, can improve production efficiency, realize automatic continuous production, reduce labor intensity, reduce energy consumption, and reduce costs.

[0006] In order to solve the above technical problems, the technical solution of the utility model is:

[0007] A device for treating the dimetholine synthesis reaction evaporation comprises an extraction tower, wherein the upper part of the extraction tower is respectively connected with a washing water pipeline and a water-containing xylene output pipeline, the washing water pipeline is provided with a water flow meter and a water regulating valve, the water-containing xylene output pipeline is connected to the water-containing xylene receiving tank; the bottom of the water-containing xylene receiving tank is connected to the lower feed port of the salt washing tower through a pipeline, a valve and a feed pump, the upper part of the salt washing tower is connected with an anhydrous xylene discharge pipeline, the anhydrous xylene discharge pipeline is connected to the anhydrous xylene receiving tank; the lower part of the extraction tower is connected with a tert-butyl alcohol xylene (synthesis reaction evaporation) feed pipeline, the tert-butyl alcohol xylene feed pipeline is provided with an evaporation flow meter and an evaporation regulating valve; the bottom of the extraction tower is connected with a water phase discharge pipe, the water phase discharge pipe is connected to the water phase receiving tank; the water flow meter, the water regulating valve, the evaporation flow meter and the evaporation regulating valve are all electrically connected to an automatic control system. A proportional control loop is formed between the water flow meter, the water regulating valve, the evaporation flow meter and the evaporation regulating valve.

[0008] Preferably, an extraction tower vent line is provided at the top of the extraction tower; a water phase vent line is provided on the water phase discharge pipe, and the tops of the extraction tower vent line and the water phase vent line are connected together.

[0009] Preferably, a water-containing xylene level gauge is provided on the side wall of the water-containing xylene receiving tank, and a water-containing xylene receiving tank venting pipeline is provided on the top; the water-containing xylene level gauge and the feed pump are interlocked and controlled with each other.

[0010] Preferably, the bottom of the salt washing tower is provided with a discharge port, the discharge port is connected to a water outlet pipe, and the water outlet pipe is provided with a water layer viewing mirror and a water layer valve. The layering of water and anhydrous xylene in the water outlet pipe is observed through the viewing mirror to avoid discharging anhydrous xylene.

[0011] Preferably, an anhydrous xylene level gauge is provided on the side wall of the anhydrous xylene receiving tank, an anhydrous xylene receiving tank venting pipeline is provided on the top, and the bottom is connected to the xylene recycling tank through a pipeline, a valve and a sleeve pump; the anhydrous xylene level gauge and the sleeve pump are interlocked and controlled with each other.

[0012] Preferably, the salt washing tower is filled with sodium chloride filler. The water in the xylene is absorbed by the salt, forming a brine with a high specific gravity and deposited at the bottom, achieving the purpose of dehydration and stratification, and separating the water in the xylene.

[0013] Preferably, a water phase receiving tank level meter is provided on the side wall of the water phase receiving tank, a water phase discharge pipe is provided at the bottom, a water phase transfer pump is provided on the water phase discharge pipe, and the water phase receiving tank level meter and the water phase transfer pump are interlocked and controlled with each other.

[0014] Preferably, the extraction tower is produced by Wuxi Hexiang Biochemical Equipment Co., Ltd., the water phase receiving tank, the aqueous xylene receiving tank and the anhydrous xylene receiving tank are all produced by Zibo Shuangte Chemical Equipment Co., Ltd.; and the dehydration salt tower is produced by Zibo Shuangte Chemical Equipment Co., Ltd.

[0015] Preferably, the automatic control system is a DCS automatic control system.

[0016] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:

[0017] The utility model automatically controls the material feed amount and feed speed of the extraction tower, so that the water and the tert-butyl alcohol-containing xylene in the extraction tower can be mixed according to the proportion, and the tert-butyl alcohol and the water are mutually dissolved and flow out from the water phase discharge pipe and enter the water phase receiving tank; the water-containing xylene from which the tert-butyl alcohol is separated is transported to the water-containing xylene receiving tank through the water-containing xylene output pipeline, and then transported to the salt washing tower for dehydration through the feed pump; the water content of the dehydrated xylene is lower than 0.1%, and the xylene is transported to the anhydrous xylene receiving tank to be further used.

[0018] In short, the utility model can improve production efficiency, realize automatic continuous production, reduce labor intensity; and can reduce energy consumption and reduce costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a structural schematic diagram of an embodiment of the utility model;

[0020] In the figure, 1. extraction tower; 2. washing water pipeline; 3. aqueous xylene output pipeline; 4. water flow meter; 5. water regulating valve; 6. aqueous xylene receiving tank; 7. feed pump; 8. salt washing tower; 9. anhydrous xylene discharge pipeline; 10. anhydrous xylene receiving tank; 11. tert-butyl alcohol xylene feed pipeline; 12. distillate flow meter; 13. distillate regulating valve; 14. aqueous phase discharge pipe; 15. aqueous phase receiving tank. DETAILED DESCRIPTION

[0021] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0022] Embodiment 1:

[0023] like Figure 1As shown, a device for treating the distillate of the oxadiazine synthesis reaction comprises an extraction tower 1, wherein the upper part of the extraction tower 1 is respectively connected with a washing water pipeline 2 and an aqueous xylene output pipeline 3, the washing water pipeline 2 is provided with a water flow meter 4 and a water regulating valve 5, the aqueous xylene output pipeline 3 is connected to an aqueous xylene receiving tank 6; the bottom of the aqueous xylene receiving tank 6 is connected to a lower feed port (not shown) of a salt washing tower 8 through a pipeline (not shown), a valve (not shown) and a feed pump 7, and the upper part of the salt washing tower 8 is connected with an anhydrous xylene output port. The extraction tower 1 is connected to a feed pipeline 9 for tert-butyl alcohol xylene, and a discharge pipeline 9 for anhydrous xylene is connected to a receiving tank 10 for anhydrous xylene. The lower part of the extraction tower 1 is connected to a feed pipeline 11 for tert-butyl alcohol xylene, and a distillate flowmeter 12 and a distillate regulating valve 13 are arranged on the feed pipeline 11 for tert-butyl alcohol xylene. The bottom of the extraction tower 1 is connected to a water phase discharge pipe 14, and the water phase discharge pipe 14 is connected to a water phase receiving tank 15. The water flowmeter 4, the water regulating valve 5, the distillate flowmeter 12 and the distillate regulating valve 13 are all electrically connected to an automatic control system (not shown).

[0024] In actual production: first, the stirring device of the extraction tower 1 and the extraction tower venting pipeline (not shown) are turned on; water enters the water flow meter 4 and the water regulating valve 5 through the washing water pipeline 2, and the water inflow is controlled by the water flow meter 4 and the water regulating valve 5; the distillate of the synthesis reaction (xylene containing tert-butyl alcohol) enters the extraction tower 1 from the bottom of the extraction tower 1 through the tert-butyl alcohol xylene feed pipeline 11 and the distillate flow meter 12 and the distillate regulating valve 13 arranged thereon, and the water and the tert-butyl alcohol xylene can be adjusted according to the proportion; the water and the tert-butyl alcohol xylene are fully mixed in the extraction tower 1, and the tert-butyl alcohol and the water are dissolved in each other and then flow out from the water phase discharge pipe 14 and enter the water phase receiving tank 15, and when the liquid level is set, it is pumped away by the water phase pump (not shown) for treatment;

[0025] The water-containing xylene is transported to the water-containing xylene receiving tank 6 through the water-containing xylene output pipeline 3, and then transported to the salt washing tower 8 through the feed pump 7. The salt washing tower 8 is filled with sodium chloride filler; the water in the xylene is precipitated by the sodium chloride to form a brine with a high specific gravity and settle to the bottom of the salt washing tower 8. The water layer valve is opened regularly to discharge the brine. The brine can be stored separately or transported to the water phase receiving tank 15. The dehydrated xylene flows out from the top of the salt tower, and the water content therein is ≤0.1%; it is transported to the water-free xylene receiving tank 10 through the anhydrous xylene discharge pipeline 9. When the liquid level reaches a certain height, the anhydrous xylene is pumped away by the application pump (not shown) for application.

[0026] It should be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the claims attached to this application.

Claims

1. A device for treating the dimetholine synthesis reaction evaporation product, characterized in that: The invention comprises an extraction tower, wherein the upper part of the extraction tower is respectively connected with a washing water pipeline and an aqueous xylene output pipeline, the washing water pipeline is provided with a water flow meter and a water regulating valve, and the aqueous xylene output pipeline is connected to an aqueous xylene receiving tank; the bottom of the aqueous xylene receiving tank is connected to the lower feed port of a salt washing tower through a pipeline, a valve and a feed pump, the upper part of the salt washing tower is connected with an anhydrous xylene discharge pipeline, and the anhydrous xylene discharge pipeline is connected to the anhydrous xylene receiving tank; the lower part of the extraction tower is connected with a tert-butyl alcohol xylene feed pipeline, and the tert-butyl alcohol xylene feed pipeline is provided with a distillate flow meter and a distillate regulating valve; the bottom of the extraction tower is connected with a water phase discharge pipe, and the water phase discharge pipe is connected to the water phase receiving tank; the water flow meter, the water regulating valve, the distillate flow meter and the distillate regulating valve are all electrically connected to an automatic control system.

2. The device for treating the dimetholine synthesis reaction evaporation product according to claim 1, characterized in that: The top of the extraction tower is provided with an extraction tower venting pipeline; the water phase discharge pipe is provided with a water phase venting pipeline, and the tops of the extraction tower venting pipeline and the water phase venting pipeline are connected together.

3. The device for treating the dimethomorph synthesis reaction evaporation product according to claim 1, characterized in that: A water-containing xylene level gauge is arranged on the side wall of the water-containing xylene receiving tank, and a water-containing xylene receiving tank venting pipeline is arranged on the top; the water-containing xylene level gauge is interlocked and controlled with the feed pump.

4. The device for treating the dimethomorph synthesis reaction evaporation product according to claim 1, characterized in that: A discharge port is provided at the bottom of the salt washing tower, and the discharge port is connected with a water outlet pipe, and a water layer sight glass and a water layer valve are provided on the water outlet pipe.

5. The device for treating the dimetholine synthesis reaction evaporation product according to claim 1, characterized in that: An anhydrous xylene level gauge is provided on the side wall of the anhydrous xylene receiving tank, an anhydrous xylene receiving tank venting pipeline is provided on the top, and the bottom is connected to the xylene recycling storage tank through pipelines, valves and a sleeve pump; the anhydrous xylene level gauge and the sleeve pump are interlocked and controlled with each other.

6. The device for treating the dimethomorph synthesis reaction evaporation product according to claim 1, characterized in that: A water phase receiving tank level meter is arranged on the side wall of the water phase receiving tank, a water phase discharge pipe is arranged at the bottom, a water phase transfer pump is arranged on the water phase discharge pipe, and the water phase receiving tank level meter and the water phase transfer pump are interlocked and controlled with each other.

7. The device for treating the dimethomorph synthesis reaction evaporation product according to claim 1, characterized in that: The automatic control system is a DCS automatic control system.