Production system of spirodiclofen

Abstract

The utility model relates to a production system of spirodiclofen and belongs to the technical field of chemical equipment. The production system comprises a reaction kettle; a discharge hole in the bottom of the reaction kettle is connected with the centrifugal machine through a centrifugal machine feeding pipeline; the centrifugal machine is a lower discharging type centrifugal machine, and a scraper is arranged in the centrifugal machine. The lower outlet is connected with the temporary storage tank through a centrifugal machine discharging pipeline; an outlet in the lower part of the temporary storage tank is connected with the reaction kettle through a reaction kettle feeding pipeline; a gas pipeline is arranged at the top of the reaction kettle; a vacuum pipeline, an air pipeline and a nitrogen pipeline are respectively arranged on the gas pipeline; a centrifugal machine leaching pipeline is arranged at the top of the centrifugal machine; a waste liquid pipeline is arranged at the bottom of the centrifuge. According to the solid-liquid separation device disclosed by the utility model, a solvent and an intermediate are prevented from being exposed in the air to injure production personnel, meanwhile, the labor intensity of the production personnel is reduced, and the operation of digging and carrying solids after solid-liquid separation is not needed.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of chemical equipment, specifically relates to a production system of spirodiclofen. BACKGROUND

[0002] Spirodiclofen is a kind of quinone acid acaricide developed by Bayer Company, which has the advantages of wide mite spectrum, long persistence, low toxicity, low residue and good safety.

[0003] The existing method for synthesizing spirodiclofen is to use 3-(2,4-dichlorophenyl)-2-oxo-1-oxaspiro[4,5]dec-3-en-4-ol and 2,2-dimethylbutyryl chloride as raw materials to react in an organic solvent to obtain the target product. After the reaction is completed, the reaction liquid is washed with alkali and water, and then the target product is precipitated by cooling. After centrifugation, the solid is refined to obtain high-purity spirodiclofen. In the existing production, the material in the centrifuge needs to be dug out manually, and then transferred to the feeding port on the second floor for manual feeding operation.

[0004] Since the organic solvents used in the reaction are mainly cyclohexane, dichloromethane and toluene, these organic solvents are volatile solvents, and the generated steam can damage the respiratory mucosa and vision of humans. Long-term online operation can cause great health risks to production personnel. In addition, since the scale of spirodiclofen produced in each batch is more than 200 kg, only the operation of collecting the solid in the centrifuge brings high work intensity to the operator.

[0005] Therefore, it is necessary to improve the production system of spirodiclofen to overcome the above problems. UTILITY MODEL CONTENTS

[0006] In view of the high solvent exposure risk and high operator intensity of the existing spirodiclofen production system, the utility model provides a production system of spirodiclofen to solve the above problems. The utility model changes the existing open production system into a closed system. After the product is centrifuged, the solid can be directly scraped off from the centrifuge, and then transferred to the temporary storage tank through the pipeline. By injecting solvent into the temporary storage tank to make it into a solid-liquid mixture, and then pumping the solid-liquid mixture into the reaction kettle through the reaction kettle feeding pipe, the contact of the material and the solvent with the workshop production personnel during production is reduced, the harm of the solvent and the intermediate to the production personnel due to exposure in the air is avoided, and the labor intensity of the production personnel is also reduced. The operation of digging and transporting the solid after solid-liquid separation is not needed.

[0007] The technical scheme of the utility model is as follows:

[0008] A production system of spirodiclofen, comprising a reaction kettle; a discharge port at the bottom of the reaction kettle is connected with a centrifuge through a centrifuge feeding pipeline; the centrifuge is a bottom discharge centrifuge, which is internally provided with a scraper; a lower outlet is connected with a temporary storage tank through a centrifuge discharge pipeline; an outlet at the lower part of the temporary storage tank is connected with the reaction kettle through a reaction kettle feeding pipeline; a gas pipeline is arranged at the top of the reaction kettle, and a vacuum pipeline, an air pipeline and a nitrogen pipeline are respectively arranged on the gas pipeline; a centrifuge washing pipeline is arranged at the top of the centrifuge; and a waste liquid pipeline is arranged at the bottom of the centrifuge.

[0009] Further, the temporary storage tank is a horizontal storage tank, which is arranged to be inclined, and is inclined to the outlet at the lower part of the temporary storage tank, and the inclination angle is 5°-10°. The horizontal storage tank is selected considering the installation height. Since the temporary storage tank needs to be lower than the discharge port of the centrifuge, it is not easy to select a higher storage tank. Generally, a vertical storage tank cannot select a large-capacity storage tank due to the height problem, and the horizontal storage tank can well overcome the height problem. In addition, the solid material scraped from the centrifuge is collected in the temporary storage tank, and the solid material is mixed with the solvent added subsequently, and then is pumped into the reaction kettle for subsequent refining. The inclined arrangement can reduce the residue of the mixed solid-liquid mixture and the washing liquid.

[0010] Further, the centrifuge is an LGZ-1600 type.

[0011] Further, the reaction kettle is connected with a condenser. In the preparation and refining operation of the crude spirodiclofen, a heating process is involved, and the condenser is arranged to ensure the reflux.

[0012] Further, the condenser is a water-cooled condenser.

[0013] Further, valves are arranged on the centrifuge feeding pipeline, the reaction kettle feeding pipeline, the waste liquid pipeline, the centrifuge washing pipeline and the centrifuge discharge pipeline.

[0014] The working principle of the utility model is: after the reaction is finished, the reaction liquid is cooled and crystallized, when centrifugation is needed, the valve at the centrifuge outlet pipeline is closed, the centrifuge is started, and the reaction kettle is pressurized. After the centrifuge rotates stably, the valve at the centrifuge inlet pipeline is opened, the reaction liquid in the reaction kettle enters the centrifuge for solid-liquid separation under the action of pressure. When there is no liquid flowing out of the waste liquid pipeline, the valve at the centrifuge outlet pipeline is opened, the solid material on the centrifuge wall is scraped down by the scraper of the centrifuge, and the solid enters the temporary storage tank through the centrifuge outlet pipeline. When the solid is scraped down completely, the rotation speed of the centrifuge is reduced to the slowest, the refined solvent which has been quantified is injected from the centrifuge washing pipeline to flush the rotating drum of the centrifuge, the solid adhered to the rotating drum of the centrifuge is flushed down and flows into the temporary storage tank. A small amount of refined solvent is reserved to be used as the solvent for subsequent flushing of the temporary storage tank. Then the centrifuge inlet pipeline is closed, the pressure in the reaction kettle is extracted to negative pressure, and then the valve on the reaction kettle inlet pipeline is opened, the solid-liquid mixture in the temporary storage tank is extracted into the reaction kettle. The residual solid in the temporary storage tank and the reaction kettle inlet pipeline is flushed by the reserved small amount of refined solvent and is extracted into the reaction kettle.

[0015] The utility model has the advantages that:

[0016] The utility model is a closed system, after product centrifugation, the solid can be scraped down from the centrifuge directly, then is transferred to the temporary storage tank through the pipeline. The solvent is injected into the temporary storage tank to make it become solid-liquid mixture, and then the solid-liquid mixture is extracted into the reaction kettle through the reaction kettle inlet pipeline, so that the contact of workshop production personnel with material and solvent in the production process is reduced, the harm of solvent and intermediate to production personnel due to exposure in the air is avoided, and the labor intensity of production personnel is reduced, and the operation of digging and carrying the solid after solid-liquid separation is not needed. BRIEF DESCRIPTION OF DRAWINGS

[0017] In order to more clearly illustrate the technical scheme of the utility model, the drawings needed to be used in the description will be briefly introduced, and obviously, the drawings in the following description are only some embodiments of the utility model, and other drawings can be obtained by those skilled in the art without creative labor.

[0018] Figure 1 It is the whole structure schematic diagram of the utility model.

[0019] In the drawing, 1 is a reaction kettle, 2 is a centrifuge, 3 is a temporary storage tank, 4 is a centrifuge inlet pipeline, 5 is a reaction kettle inlet pipeline, 6 is a waste liquid pipeline, 7 is a centrifuge washing pipeline, 8 is a gas pipeline, 9 is a centrifuge outlet pipeline, and 10 is a condenser. DETAILED DESCRIPTION

[0020] In order to make the purpose, features and advantages of the utility model more obvious and easy to understand, the technical scheme of the utility model will be clearly and completely described below in combination with the drawings in the specific embodiments. Obviously, the following described embodiments are only a part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the patent, all other embodiments obtained by the ordinary skilled in the art without making creative efforts belong to the protection scope of the patent.

[0021] Embodiment 1

[0022] A production system of spirodiclofen, comprising a reaction kettle 1; a discharge port at the bottom of the reaction kettle 1 is connected with a centrifuge 2 through a centrifuge feed pipeline 4; the centrifuge 2 is a lower discharge type centrifuge, and a scraper is arranged inside; a lower outlet is connected with a temporary storage tank 3 through a centrifuge discharge pipeline 9; an outlet at the lower part of the temporary storage tank 3 is connected with the reaction kettle 1 through a reaction kettle feed pipeline 5; a gas pipeline 8 is arranged at the top of the reaction kettle 1, and a vacuum pipeline, an air pipeline and a nitrogen pipeline are respectively arranged on the gas pipeline 8; a centrifuge washing pipeline 7 is arranged at the top of the centrifuge 2; a waste liquid pipeline 6 is arranged at the bottom of the centrifuge 2.

[0023] Embodiment 2

[0024] A production system of spirodiclofen, comprising a reaction kettle 1; a discharge port at the bottom of the reaction kettle 1 is connected with a centrifuge 2 through a centrifuge feed pipeline 4; the centrifuge 2 is a lower discharge type centrifuge, and a scraper is arranged inside; a lower outlet is connected with a temporary storage tank 3 through a centrifuge discharge pipeline 9; an outlet at the lower part of the temporary storage tank 3 is connected with the reaction kettle 1 through a reaction kettle feed pipeline 5; the temporary storage tank 3 is a horizontal storage tank, and is arranged to be inclined, and is inclined to the outlet direction at the lower part of the temporary storage tank 3, and the inclination angle is 5°; a gas pipeline 8 is arranged at the top of the reaction kettle 1, and a vacuum pipeline, an air pipeline and a nitrogen pipeline are respectively arranged on the gas pipeline 8; a centrifuge washing pipeline 7 is arranged at the top of the centrifuge 2; a waste liquid pipeline 6 is arranged at the bottom of the centrifuge 2; the reaction kettle 1 is connected with a condenser 10; the condenser 10 is a water-cooled condenser; and valves are arranged on the centrifuge feed pipeline, the reaction kettle feed pipeline, the waste liquid pipeline, the centrifuge washing pipeline and the centrifuge discharge pipeline.

[0025] The above description of the disclosed embodiments enables a person skilled in the art to implement or use the utility model. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the utility model. Therefore, the utility model will not be limited to these embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A production system of spirodiclofen, comprising a reaction kettle; a discharge port at the bottom of the reaction kettle is connected with a centrifuge through a centrifuge feeding pipeline; characterized in that, The centrifuge is a bottom discharge centrifuge, which is internally provided with a scraper; a lower outlet is connected with a temporary storage tank through a centrifuge discharge pipeline; an outlet at the lower part of the temporary storage tank is connected with a reaction kettle through a reaction kettle feed pipeline; a gas pipeline is arranged at the top of the reaction kettle, and a vacuum pipeline, an air pipeline and a nitrogen pipeline are respectively arranged on the gas pipeline; a centrifuge rinsing pipeline is arranged at the top of the centrifuge; and a waste liquid pipeline is arranged at the bottom of the centrifuge.

2. The production system of a spirodiclofen according to claim 1, wherein, The temporary storage tank is a horizontal storage tank, which is arranged in an inclined manner and is inclined to the outlet direction at the lower part of the temporary storage tank, and the inclination angle is 5°-10°.

3. The production system of the spiromesifen according to claim 1, wherein The centrifuge model is LGZ-1600.

4. The production system of the spiromesifen according to claim 1, wherein The reaction kettle is connected with a condenser.

5. The production system of a spirodiclofen according to claim 4, wherein the step of adding the organic solvent is performed after the step of adding the acid. The condenser is a water-cooled condenser.

6. The production system of a spirodiclofen according to claim 1, wherein Valves are arranged on the centrifuge feed pipeline, the reaction kettle feed pipeline, the waste liquid pipeline, the centrifuge rinsing pipeline and the centrifuge discharge pipeline.

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