Low-content chlorothalonil refining device
By setting up a dissolving tank, a washing tank, a decolorizing tank, a crystallizing tank, and a reflux toluene-removing tank, combined with filtration and separation steps, the problems of low yield and high cost in the production of chlorothalonil were solved, and a highly efficient refining process was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-02
- Publication Date
- 2026-03-27
AI Technical Summary
In the process of large-scale continuous production of chlorothalonil, it is impossible to find the optimal process conditions immediately, resulting in more side reactions, incomplete reactions, reduced product yield, high hexachlorobenzene content, and increased costs.
The process employs a dissolving vessel, a washing vessel, a decolorizing vessel, a crystallizing vessel, and a reflux toluene-removing vessel. Through multiple steps of filtration and separation using filters and separation components, combined with a stirring motor, temperature control, and a transfer pump, a refining process is achieved.
It improved product yield, reduced hexachlorobenzene content, reduced solid waste, and lowered production costs.
Smart Images
Figure CN224040566U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the technical field of chemical production equipment, concretely relates to a low content chipton refining device. BACKGROUND
[0002] Chipton is a high -efficient low -toxic broad -spectrum fungicide, and its main role is to prevent crops from being infected by fungi, and also be used as industrial antifungal agent, fruit preservative and protective agent of coating and adhesive. And the chipton of commercialization has the requirement in content, color and crystal form, and the content of impurity hexachlorobenzene (HCB) needs less than 10ppm.
[0003] In the actual mass (ten thousand tons level production capacity) continuous production process, various process parameters need to be debugged and optimized in the starting stage, such as reaction temperature, pressure, raw material ratio, reaction time etc.;In the process of parameter adjustment, due to the fact that the best process condition cannot be found immediately, the reaction cannot be carried out in the ideal state, thereby producing more side reactions or incomplete reactions, and then producing the post-catch material with content of 60-80%, and the content of hexachlorobenzene (HCB) is high (400-700ppm), and the color presents yellow or green, resulting in the reduction of product yield and the rise of production cost. UTILITY MODEL CONTENT
[0004] The utility model discloses a low content chipton refining device.
[0005] The utility model discloses a low content chipton refining device.
[0006] The dissolution kettle, the water washing kettle, the decoloring kettle, the crystallization kettle and the reflux methylbenzene cutting kettle are communicated through pipelines;
[0007] The first filter is arranged between the dissolution kettle and the water washing kettle, the second filter is arranged between the decoloring kettle and the crystallization kettle, and the third filter is arranged between the crystallization kettle and the reflux methylbenzene cutting kettle.
[0008] The first feeding port is arranged on the top of the dissolution kettle, one group of first feeding ports is communicated with the first feeding bin through a pipeline, the first discharge port is arranged at the bottom of the dissolution kettle, and the first discharge port is communicated with the first filter through a pipeline.
[0009] The second feeding port is arranged on the top of the water washing kettle, one group of second feeding ports is communicated with the first filter through a pipeline, the second discharge port is arranged at the bottom of the water washing kettle, and the second discharge port is communicated with the decoloring kettle through a pipeline.
[0010] As the further description of the above technical scheme, the third feeding port is arranged on the top of the decoloring kettle, a group of the third feeding ports are communicated with the second feeding bin through pipelines, the third discharging port is arranged on the bottom of the dissolving kettle, and the third discharging port is communicated with the second filter through a pipeline.
[0011] As the further description of the above technical scheme, the first filter port is arranged on one side of the first filter, the first filter port is communicated with the dissolving kettle through a pipeline, the first filter port is arranged on the bottom of the first filter, and the first filter port is communicated with the dissolving kettle through a pipeline.
[0012] As the further description of the above technical scheme, the second filter port is arranged on one side of the second filter, the second filter port is communicated with the decoloring kettle through a pipeline, the second filter port is arranged on the bottom of the second filter, and the second filter port is communicated with the crystallization kettle through a pipeline.
[0013] As the further description of the above technical scheme, the fourth feeding port is arranged on one side of the top of the crystallization kettle, the fourth feeding port is communicated with the second filter through a pipeline, the fourth discharging port is arranged on the bottom of the crystallization kettle, and the fourth discharging port is communicated with the third filter through a pipeline.
[0014] As the further description of the above technical scheme, the third filter port is arranged on one side of the top of the third filter, the third filter port is communicated with the crystallization kettle through a pipeline, the third filter port is arranged on the bottom of the third filter, and the third filter port is communicated with the reflux methylbenzene cutting kettle through a pipeline.
[0015] As the further description of the above technical scheme, the first material transferring pump is arranged on the pipeline communicated between the water washing kettle and the decoloring kettle, and the second material transferring pump is arranged on the pipeline communicated between the third filter and the reflux methylbenzene cutting kettle.
[0016] As the further description of the above technical scheme, the separation assembly comprises a condenser, a water distributor and a centrifugal machine, the fifth feeding ports are arranged on the top of the reflux methylbenzene cutting kettle, a group of the fifth feeding ports are communicated with the third filter through pipelines, a group of the fifth feeding ports are communicated with the centrifugal machine through pipelines, a group of the fifth feeding ports are communicated with the condenser through pipelines, the condenser is communicated with the water distributor through a pipeline, a group of the fifth feeding ports are communicated with the water distributor through pipelines, and the fifth discharging port is arranged on the bottom of the crystallization kettle and communicated with the centrifugal machine through a pipeline.
[0017] The beneficial effects of the utility model are as follows:
[0018] The utility model discloses, be provided with dissolving cauldron, water washing cauldron, decoloring cauldron, crystallization cauldron and reflux cut toluene cauldron, complete dissolving, filtration, water washing layering, decoloring and cooling crystallization process in proper order, and then the post-trapping material produced in the stage of starting is refined and purified, can effectively reduce solid waste amount and reduce production cost while improving product yield.
[0019] In order to more clearly set forth the structural features and effects of the utility model, the utility model will be described in detail below in conjunction with the drawings and specific embodiments. BRIEF DESCRIPTION OF DRAWINGS
[0020] Figure 1 It is the structure schematic diagram of low content of the utility model for refining chlorothalonil device.
[0021] Reference signs:
[0022] 1, dissolving cauldron, 101, first feed inlet, 102, first discharge port, 2, water washing cauldron, 201, second feed inlet, 202, second discharge port, 3, decoloring cauldron, 301, third feed inlet, 302, third discharge port, 4, crystallization cauldron, 401, fourth feed inlet, 402, fourth discharge port, 5, reflux cut toluene cauldron, 501, fifth feed inlet, 502, fifth discharge port, 6, first filter, 601, first filter inlet, 602, first filter outlet, 7, second filter, 701, second filter inlet, 702, second filter outlet, 8, third filter, 801, third filter inlet, 802, third filter outlet, 9, first feeding bin, 10, second feeding bin, 11, condenser, 12, water segregator, 13, centrifuge. DETAILED DESCRIPTION
[0023] In order to make the purpose, technical scheme and advantage of the utility model embodiment more clearly, the technical scheme in the utility model embodiment will be clearly and completely described below in conjunction with the drawings in the utility model embodiment.
[0024] As Figure 1 Indicated, in an embodiment, a low content of the utility model for refining chlorothalonil device, include: through the pipeline intercommunication of dissolving cauldron, water washing cauldron, decoloring cauldron, crystallization cauldron and reflux cut toluene cauldron, wherein, between dissolving cauldron and water washing cauldron are provided with first filter, and between decoloring cauldron and crystallization cauldron are provided with second filter, and between crystallization cauldron and reflux cut toluene cauldron are provided with third filter, for the filtrating of dissolved liquid step by step multiple times.
[0025] The dissolving kettle is used for heating, dissolving and stirring the toluene and low content of chlorothalonil put into the kettle, and then the toluene and low content of chlorothalonil are conveyed to the water washing kettle after the solid insoluble substances are filtered out through the first filter; the water washing kettle is used for washing the filtrate by adding water, and the organic phase liquid is conveyed to the decolorizing kettle after the water phase is separated; the decolorizing kettle is used for adsorbing the liquid by adding activated carbon, and then the liquid is conveyed to the crystallizing kettle after the solid insoluble substances are filtered out through the second filter; and the crystallizing kettle is used for cooling the liquid, and then the product is filtered out through the third filter and conveyed to the toluene recovery kettle.
[0026] It can be understood that the dissolving kettle, the water washing kettle, the decolorizing kettle, the crystallizing kettle and the toluene recovery kettle are all provided with stirring motors at the top, and the stirring motors are rotationally connected with stirring paddles in the kettles, and each kettle is provided with a thermometer and a heating jacket (not shown in the figure) to monitor the temperature in the kettle.
[0027] It needs to be particularly pointed out that the toluene recovery kettle is connected with the separation assembly composed of the condenser, the water separator and the centrifugal machine through pipelines, so that the toluene as a solvent can be evaporated, condensed and collected and conveyed to the toluene storage tank.
[0028] Please continue to refer to Figure 1 In the embodiment, the dissolving kettle 1 is provided with a first feeding port 101 at the top of each side, and one group of the first feeding ports 101 is used for putting toluene, and the other group of the first feeding ports 101 is connected with the first feeding bin 9 through pipelines and used for putting low content of chlorothalonil; correspondingly, the dissolving kettle 1 is provided with a first discharging port 102 at the bottom, and the first discharging port 102 is connected with the first filter 6 through pipelines, so that the dissolved liquid can be conveyed to the first filter 6.
[0029] Further, the first filter 6 is provided with a first filtering port 601 at one side, and the first filtering port 601 is connected with the dissolving kettle 1 through pipelines and used for receiving the liquid and filtering out insoluble solids; correspondingly, the first filter 6 is provided with a first filtering port 602 at the bottom, and the first filtering port 602 is connected with the water washing kettle 2 through pipelines, so that the filtered liquid can be conveyed to the water washing kettle 2. Specifically, the first filter can be a basket filter.
[0030] Further, the water washing kettle 2 is provided with a second feeding port 201 at the top of each side, and one group of the second feeding ports 201 is used for putting water, and the other group of the second feeding ports 201 is connected with the first filter 6 through pipelines; correspondingly, the water washing kettle 2 is provided with a second discharging port 202 at the bottom, and the second discharging port 202 is connected with the decolorizing kettle 3 through pipelines, so that the organic phase liquid after the layering can be conveyed to the decolorizing kettle 3. Specifically, the pipeline connected with the water washing kettle 2 and the decolorizing kettle 3 is provided with a first liquid transferring pump.
[0031] Further, the third feeding port 301 is arranged on the top of the decoloring kettle 3, and a group of the third feeding port 301 is communicated with the water washing kettle 2 through a pipeline, and another group of the third feeding port 301 is communicated with the second feeding bin 10 through a pipeline, for feeding activated carbon; correspondingly, the third discharging port 302 is arranged at the bottom of the dissolving kettle 1, and the third discharging port 302 is communicated with the second filter 7 through a pipeline, so that the adsorbed liquid can be transported into the second filter 7.
[0032] Further, the second filter 7 is provided with the second filtering inlet 701 on one side, and the second filtering inlet 701 is communicated with the decoloring kettle 3 through a pipeline, for receiving the liquid and filtering out the insoluble solids in the liquid; correspondingly, the second filter 7 is provided with the second filtering outlet 702 at the bottom, and the second filtering outlet 702 is communicated with the crystallization kettle 4 through a pipeline, so that the filtered liquid can be transported into the crystallization kettle 4. Specifically, the second adsorber can adopt a basket filter.
[0033] Further, the crystallization kettle 4 is provided with the fourth feeding port 401 on one side of the top, and the fourth feeding port 401 is communicated with the second filter 7 through a pipeline; correspondingly, the crystallization kettle 4 is provided with the fourth discharging port 402 at the bottom, and the fourth discharging port 402 is communicated with the third filter 8 through a pipeline, so that the crystallized liquid can be transported into the third filter 8.
[0034] Further, the third filter 8 is provided with the third filtering inlet 801 on one side of the top, and the third filtering inlet 801 is communicated with the crystallization kettle 4 through a pipeline; correspondingly, the third filter 8 is provided with the third filtering outlet 802 at the bottom, and the third filtering outlet 802 is communicated with the reflux cut toluene kettle 5 through a pipeline. Specifically, the third adsorber can adopt a two-in-one filter; and the pipeline communicated between the third filter 8 and the reflux cut toluene kettle 5 is provided with a second material transfer pump.
[0035] Further, the reflux cut toluene kettle 5 is provided with the fifth feeding port 501 on both sides of the top, wherein a group of the fifth feeding port 501 is communicated with the third filter 8 through a pipeline, a group of the fifth feeding port 501 is communicated with the centrifugal machine 13 through a pipeline, a group of the fifth feeding port 501 is communicated with the condenser 11 through a pipeline, the condenser 11 is communicated with the water distributor 12 through a pipeline, and a group of the fifth feeding port 501 is communicated with the water distributor 12 through a pipeline, so as to form a condensation and cutting circulation loop, toluene is evaporated and condensed into a toluene recovery tank for collection, and water continues to be fed into the reflux cut toluene; correspondingly, the crystallization kettle 4 is provided with the fifth discharging port 502 at the bottom, and the fifth discharging port 502 is communicated with the centrifugal machine 13 through a pipeline, for filtering out the insoluble solids in the liquid after the toluene collection is completed.
[0036] Working principle: low content of chlorothalonil is placed in the first feeding bin 9, activated carbon is placed in the second feeding bin 10, then low content of chlorothalonil and toluene are respectively put into the dissolving kettle 1 through the first feeding port 101, after heating, dissolving and fully stirring, the filtrate is filtered through the first filter 6 to remove insoluble solids, and then transported to the water washing kettle 2, then water is added through the intermittent feeding port to stir and stand to separate layers, so that the organic phase layer (toluene layer) can be transported to the decolorization kettle 3 through the first transfer pump, then activated carbon is put into the decolorization kettle 3 through the second feeding port 201, after heating and fully stirring, the filtrate is filtered through the second filter 7 to remove insoluble solids, and then transported to the crystallization kettle 4, after cooling and crystallization, the solid product is filtered through the third filter 8, and then dried to determine the content, while the toluene filtrate is transported to the reflux toluene kettle 5 through the second transfer pump, after adding water and heating, the toluene is cut off through the water separator 12 after cooling through the condenser 1, and then collected and recovered to the toluene storage tank, after the toluene recovery is completed, the filtrate is transported to the centrifuge 13, and then the water is recovered to the reflux toluene kettle 5 for continuous use, the recovered toluene can also be continuously used in the solvent kettle, and the insoluble solids filtered in all steps are collected and then incinerated in the regenerative thermal oxidizer (RTO) system.
[0037] The application also provides a low-content chlorothalonil refining process, and the specific steps are as follows:
[0038] S100: low-content chlorothalonil and toluene are put into the dissolving kettle 1, heated and dissolved at a preset temperature, then filtered through nitrogen to remove solid insoluble substances through the first filter 6 while hot, and the liquid is transported to the water washing kettle 2;
[0039] S200: water is added to the water washing kettle 2, washed at a preset temperature, and then separated into water phase after standing, and the organic phase liquid is transported to the decolorization kettle 3;
[0040] S300: activated carbon is added to the decolorization kettle 3, fully stirred at a preset temperature, then filtered through nitrogen to remove solid insoluble substances through the second filter 7 while hot, and the liquid is transported to the crystallization kettle 4;
[0041] S400: slowly cool in the crystallization kettle 4, so that the temperature decreases to a preset temperature, then filter the solid product through the third filter 8 by filtering the liquid through nitrogen, the filtrate is transported to the recovery toluene kettle, and the solid product is transferred to the dryer for drying and content determination;
[0042] S500: After adding water to the filtrate in the recovery cut toluene kettle, start heating and distillation, after cooling, through the water trap 12, recover to the toluene storage tank, the separated water is continuously transported to the recovery cut toluene kettle for continuous use, after the toluene is completely distilled out, the filtrate is pressure filtered into the centrifuge 13 by nitrogen to remove the solid insoluble matter, the remaining water is collected and transported to the recovery water kettle for continuous use.
[0043] It needs to be explained in detail that all the solid insoluble matters filtered in the steps are collected and then enter the regenerative thermal incinerator for incineration treatment.
[0044] Exemplarily, the mass ratio of low content of chlorothalonil to toluene is 1:2-10 (preferably 1:3-5);
[0045] Further, the mass ratio of water added in the water washing kettle 2 to low content of chlorothalonil is 0.001-0.1:1 (preferably 0.005-0.1:1);
[0046] Further, the mass ratio of activated carbon added in the decolorization kettle 3 to low content of chlorothalonil is 0.005-0.05:1 (preferably 0.01-0.05:1);
[0047] Further, the cooling rate in the crystallization kettle is 5-20 ℃ / h (preferably 8-10 ℃ / h).
[0048] Example 1
[0049] 75% of the post-capture chlorothalonil 1000 kg is added to toluene 4000 kg for heating and dissolution, after hot filtration, 80 kg of water is added for sufficient stirring, after static stratification, the toluene layer is transferred to the decolorization kettle 3, 40 kg of activated carbon is added, and then filtered, the filtrate is transferred to the crystallization kettle 4, and the temperature is reduced to 25 ℃ or below, and then centrifuged, and the chlorothalonil solid is dried.
[0050] The filtrate is transferred to the reflux cut toluene kettle 5 for azeotropic distillation, and after the water is separated by the water trap 12, the toluene is transferred to the recovery toluene storage tank. The water is re-transferred to the reflux cut toluene kettle 5 for continuous use. After the toluene recovery is completed, the liquid is transferred to the centrifuge 13 for centrifugation, and the recovered water is continuously used. The recovered toluene is transferred to the dissolution kettle 1 for use.
[0051] Example 2
[0052] In this example, the difference from example 1 is that the content of post-capture chlorothalonil is 60%, and 100 kg of water is added to the stratification kettle.
[0053] Example 3
[0054] In this example, the difference from example 1 is that the mass of toluene is 4500 kg, and 100 kg of water is added to the stratification kettle.
[0055] Example 4
[0056] In this example, the difference from Example 1 is that the activated carbon mass is 50 kg and the crystallization rate is 5℃ / h.
[0057] Example 5
[0058] In this example, the difference from Example 1 is that the content of the post-trapped chlorothalonil is 80% and the mass of toluene is 3500 kg.
[0059] Example 6
[0060] In this example, the difference from Example 1 is that the content of the post-trapped chlorothalonil is 80% and 50 kg of water is added to the layered tank.
[0061] Example 7
[0062] In this example, the difference from Example 1 is that the mass of toluene is 5000 kg and the mass of activated carbon is 10 kg.
[0063] Example 8
[0064] In this example, the difference from Example 1 is that the mass of toluene is 5000 kg and the crystallization rate is 15℃ / h.
[0065] Example 9
[0066] In this example, the difference from Example 1 is that 80 kg of water is added to the layered tank and the crystallization rate is 8℃ / h.
[0067] Table 1: Summary of product quality, detection and yield of refined chlorothalonil after Examples 1-9
[0068]
[0069] As can be seen from the above table, the technical scheme of the present application can refine and purify the post-trapped material generated during the start-up stage. The content of the post-chlorothalonil product after treatment by the above refining equipment and refining process is greater than 98.50%, the content of hexachlorobenzene (HCB) is low (2-8 ppm), and the yield can reach more than 90%. The product yield can be improved, the amount of solid waste can be effectively reduced, and the production cost can be reduced.
[0070] The above description of disclosed embodiments enables one of ordinary skill in the art to make or use the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein can be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A low content of chlorothalonil refining device, characterized by, The utility model relates to a kind of production device of methylbenzene, including: Dissolution kettle, water washing kettle, decoloring kettle, crystallization kettle and reflux methylbenzene kettle are communicated by pipeline; First filter is arranged between the dissolution kettle and the water washing kettle, second filter is arranged between the decoloring kettle and the crystallization kettle, third filter is arranged between the crystallization kettle and the reflux methylbenzene kettle, the reflux methylbenzene kettle is communicated with separation assembly by pipeline, and the separation assembly is used to separate product.
2. The low content of chlorothalonil refining device according to claim 1, characterized in that, First feeding port is arranged on the top of the dissolution kettle, a group of first feeding ports are communicated with first feeding bin by pipeline, first discharge port is arranged on the bottom of the dissolution kettle, and the first discharge port is communicated with first filter by pipeline.
3. The low content of chlorothalonil refining device according to claim 2, characterized in that, Second feeding port is arranged on the top of the water washing kettle, a group of second feeding ports are communicated with first filter by pipeline, second discharge port is arranged on the bottom of the water washing kettle, and the second discharge port is communicated with decoloring kettle by pipeline.
4. The low content of chlorothalonil refining device according to claim 3, characterized in that, Third feeding port is arranged on the top of the decoloring kettle, a group of third feeding ports are communicated with second feeding bin by pipeline, third discharge port is arranged on the bottom of the dissolution kettle, and the third discharge port is communicated with second filter by pipeline.
5. The low content of chlorothalonil refining device according to claim 3, characterized in that, First filter port is arranged on one side of the first filter, and the first filter port is communicated with dissolution kettle by pipeline.
6. The low content of chlorothalonil refining device according to claim 4, characterized in that, Second filter port is arranged on one side of the second filter, and the second filter port is communicated with decoloring kettle by pipeline.
7. The low content of chlorothalonil purification device according to claim 6, characterized in that, Fourth feeding port is arranged on one side of the top of the crystallization kettle, and the fourth feeding port is communicated with second filter by pipeline.
8. The low content of chlorothalonil purification device according to claim 7, characterized in that, Third filter port is arranged on one side of the top of the third filter, and the third filter port is communicated with crystallization kettle by pipeline.
9. The low content of chlorothalonil refining device according to claim 1, characterized in that, First transfer pump is arranged on the pipeline communicated with the water washing kettle and the decoloring kettle, and second transfer pump is arranged on the pipeline communicated with the third filter and the reflux methylbenzene kettle.
10. The low content of chlorothalonil refining apparatus according to claim 1, characterized in that, The separation assembly includes condenser, water distributor and centrifuge, fifth feeding port is arranged on both sides of the top of the reflux methylbenzene kettle, a group of fifth feeding ports are communicated with third filter by pipeline, a group of fifth feeding ports are communicated with centrifuge by pipeline, a group of fifth feeding ports are communicated with condenser by pipeline, condenser is communicated with water distributor by pipeline, a group of fifth feeding ports are communicated with water distributor by pipeline, and fifth discharge port is arranged on the bottom of the crystallization kettle, and the fifth discharge port is communicated with centrifuge by pipeline.