Production device for isoxadifen-ethyl acid intermediate

Abstract

The utility model relates to a production device for an isoxadifen-ethyl intermediate, and belongs to the technical field of chemical equipment. An outlet of the sodium hypochlorite storage tank is connected with a high-level tank, and outlet ends of the high-level tank, the benzophenone hydrazone feeding tank and the dichloromethane storage tank are connected with the synthesis kettle through pipelines; transfer pumps are arranged between the sodium hypochlorite storage tank and the high-level tank and between the dichloromethane storage tank and the synthesis kettle; a flow control valve is arranged between the high-level tank and the synthesis kettle; the lower part of the synthesis kettle is sequentially connected with a kettle bottom valve and a filtering centrifugal machine through pipelines, the bottom of the filtering centrifugal machine is connected with a solid waste packing machine, the side surface of the centrifugal machine is connected with a transfer pump and a distillation kettle, a lower outlet of the distillation kettle is connected with a product storage tank, and an upper outlet of the distillation kettle is connected with a dichloromethane recovery tank. According to the device provided by the utility model, the feeding is convenient, the solvent is recycled after being distilled, the utilization rate of the solvent can be effectively improved, the production cost is saved, and the waste discharge is reduced.

Description

Technical Field

[0001] The utility model relates to a production device for an intermediate of bispyribac-sodium, belonging to the technical field of chemical equipment. Background Art

[0002] Bispyribac-sodium is a safe herbicide for plants, mainly used for weeding in corn fields and paddy fields. Herbicidal products containing bispyribac-sodium include nicosulfuron, rimsulfuron, mesosulfuron-methyl, mesotrione, and quizalofop-p-ethyl. In the production process of bispyribac-sodium, benzophenone hydrazone and sodium hypochlorite are used as raw materials for reaction, and dichloromethane is used as a solvent to obtain an intermediate (azodiphenylmethane). Currently, there is no special supporting equipment for this process, and manual operation is required. In particular, sodium hypochlorite is prone to overdose during the addition process, resulting in too many by-products. After the reaction, the solvent cannot be recovered well, causing environmental pollution and waste of resources. Summary of the Invention

[0003] In order to make up for the deficiencies of the prior art, the utility model provides a production device for an intermediate of bispyribac-sodium.

[0004] In order to achieve the above purpose, the utility model is realized by adopting the following technical scheme:

[0005] A production device for an intermediate of bispyribac-sodium, including a device body, the device body includes a benzophenone hydrazone feeding tank, a sodium hypochlorite storage tank, a dichloromethane storage tank and a synthesis kettle; the outlet of the sodium hypochlorite storage tank is connected to a high-level tank through a pipeline, and the high-level tank, the benzophenone hydrazone feeding tank and the outlet ends of the dichloromethane storage tank are all connected to the synthesis kettle through pipelines; transfer pumps are arranged between the sodium hypochlorite storage tank and the high-level tank, and between the dichloromethane storage tank and the synthesis kettle, and a flow control valve is arranged between the high-level tank and the synthesis kettle; the lower part of the synthesis kettle is sequentially connected to a bottom valve and a filter centrifuge through pipelines, the bottom of the filter centrifuge is connected to a solid waste baler, a transfer pump and a distillation kettle are connected to the side of the centrifuge, the lower outlet of the distillation kettle is connected to a product storage tank, and the upper outlet of the distillation kettle is connected to a dichloromethane recovery tank.

[0006] Preferably, the bottom position of the benzophenone hydrazone feeding tank is higher than the top end of the synthesis kettle.

[0007] Preferably, the outlet of the dichloromethane recovery tank is connected to a circulation pump, and the other end of the circulation pump is connected to the dichloromethane storage tank through a pipeline.

[0008] Compared with the prior art, the advantages and positive effects of the utility model are as follows:

[0009] 1. The device provided by the utility model is convenient for feeding. After the sodium hypochlorite is raised, it can, under the action of gravity, control the dropping rate through a valve to prevent overdose, effectively control the reaction process, and reduce the generation of by-products.

[0010] 2. After discharging, through a centrifuge and an automatic waste baler, solid waste can be effectively separated, manual operation is reduced, and pollution is lowered.

[0011] 3. The solvent is recovered and reused after distillation, which can effectively improve the utilization rate of the solvent, save production costs, and reduce waste emissions. Description of the Drawings

[0012] Figure 1 It is a schematic structural diagram of the utility model.

[0013] Each reference numeral is: 1 benzophenone hydrazone feeding tank, 2 sodium hypochlorite storage tank, 3 elevated tank, 4 synthesis kettle, 5 dichloromethane storage tank, 6 filter centrifuge, 7 solid waste baler, 8 distillation kettle, 9 product storage tank, 10 dichloromethane recovery tank, 11 circulation pump. Detailed Embodiments

[0014] In order to more clearly understand the above-mentioned objects, features, and advantages of the utility model, the following further describes the utility model with reference to the drawings and embodiments. It should be noted that, without conflict, the embodiments of the present application and the features in the embodiments can be combined with each other.

[0015] In the following description, many specific details are set forth to fully understand the utility model. However, the utility model can also be implemented in other ways different from those described herein. Therefore, the utility model is not limited by the specific embodiments disclosed in the following specification.

[0016] Embodiment 1

[0017] The drawing is a specific embodiment of the utility model. In this embodiment, without special description, the conventional devices and processes for the production of bisbenzoxazole acid intermediates are used. As Figure 1As shown in the figure, the present embodiment provides a production device for the intermediate of bisbenzoxazolic acid, including storage components for three raw materials, namely, the benzophenone hydrazone feeding tank 1 (dust-free feeding), the sodium hypochlorite storage tank 2, and the dichloromethane storage tank 5, all of which are connected to different inlets of the synthesis kettle 4 through pipelines. Among them, the horizontal position of the benzophenone hydrazone feeding tank 1 is higher than that of the synthesis kettle 4, so that the solid materials can smoothly enter the synthesis kettle 4 under the action of gravity. The horizontal positions of the sodium hypochlorite storage tank 2 and the dichloromethane storage tank 5 are both lower than that of the synthesis kettle 4. A material pump is arranged between the dichloromethane storage tank 5 and the synthesis kettle 4, and between the sodium hypochlorite storage tank 2 and the high-level tank 3; the horizontal position of the high-level tank 3 is also higher than that of the synthesis kettle 4, and a flow control valve for controlling the dropping rate of sodium hypochlorite is arranged between the high-level tank 3 and the synthesis kettle 4. All three materials enter from the upper part or the top of the synthesis kettle 4. In order to meet the reaction requirements, the synthesis kettle 4 itself is equipped with a heating jacket and a stirring mechanism. In addition, an exhaust pipeline and a sampling pipeline are arranged at the upper part of the synthesis kettle 4. The reaction is judged whether it meets the requirements through sampling detection. The above-mentioned structures of the synthesis kettle 4 are the conventional structures of industrial synthesis kettles, which can be customized by manufacturers according to needs, and the reaction conditions remain unchanged. This will not be elaborated here in this embodiment. A bottom valve is arranged at the lower part of the synthesis kettle 4, and a filter centrifuge 6 is arranged below the bottom valve. The bottom of the filter centrifuge 6 is connected to the inlet of an automatic solid waste baler 7 through a relatively thick pipeline, and the side of the filter centrifuge 6 is connected to a transfer pump and a distillation kettle 8 through a pipeline. The bottom valve is closed during the synthesis reaction, and the reaction is intermittent. After the reaction is completed, the bottom valve is opened. The materials enter the filter centrifuge 6 arranged at the lower part of the synthesis kettle 4 under the action of gravity. The materials after centrifugation by the filter centrifuge 6 are divided into two parts: the solid is waste, which enters the solid waste baler 7 under the action of gravity for waste treatment; the liquid is thrown out into the discharge pipe and then enters the distillation kettle 8 for further separation. A product storage tank 9 is arranged at the lower part of the distillation kettle 8, and the target product azodibenzylmethane is obtained at the lower part of the distillation kettle 8; the outlet pipeline at the upper part of the distillation kettle 8 is connected to a dichloromethane recovery tank 10, and the outlet of the dichloromethane recovery tank 10 is connected to a circulation pump 11 through a pipeline, and the other end of the circulation pump 11 is connected to the dichloromethane storage tank 5 through a pipeline. The solvent dichloromethane obtained by distillation can be directly replenished into the dichloromethane storage tank 5 for repeated use.

[0018] The above is only the preferred embodiment of the present invention, and it is not a limitation to the present invention in other forms. Any person skilled in the art may use the disclosed technical content to make changes or modifications into equivalent embodiments with equivalent changes and apply them to other fields. However, as long as it does not depart from the technical content of the technical solution of the present invention, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims

1. A production device for an isoxadifen intermediate, comprising a device body, characterized in that: The device body comprises a benzophenone hydrazone feeding tank, a sodium hypochlorite storage tank, a dichloromethane storage tank and a synthesis kettle; the outlet of the sodium hypochlorite storage tank is connected to a high-level tank through a pipeline, and the high-level tank, the benzophenone hydrazone feeding tank and the outlet end of the dichloromethane storage tank are all connected to the synthesis kettle through pipelines; a material transfer pump is arranged between the sodium hypochlorite storage tank and the high-level tank, and between the dichloromethane storage tank and the synthesis kettle, and a flow control valve is arranged between the high-level tank and the synthesis kettle; the lower part of the synthesis kettle is connected to a kettle bottom valve and a filtering centrifuge through pipelines in sequence, the bottom of the filtering centrifuge is connected to a solid waste baler, the side of the centrifuge is connected to a material transfer pump and a distillation kettle, the lower outlet of the distillation kettle is connected to a product storage tank, and the upper outlet of the distillation kettle is connected to a dichloromethane recovery tank.

2. The production device for isoxadifen intermediate according to claim 1, characterized in that: The bottom of the benzophenone hydrazone feeding tank is higher than the top of the synthesis reactor.

3. The production device for isoxadifen intermediate according to claim 1, characterized in that: The outlet of the dichloromethane recovery tank is connected to a circulation pump, and the other end of the circulation pump is connected to the dichloromethane storage tank through a pipeline.

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