1, 4-naphthoquinone purification device

Abstract

The utility model discloses a 1, 4-naphthoquinone purification device, and relates to the technical field of 1, 4-naphthoquinone production, an outlet of a 1, 4-naphthoquinone solution tank is communicated with a sublimation kettle, a top outlet of the sublimation kettle is communicated with a receiving kettle, and a bottom outlet of the receiving kettle is respectively communicated with a solvent receiving tank and a 1, 4-naphthoquinone product tank. The 1, 4-naphthoquinone solution is heated to 60 DEG C, the solvent is evaporated out and enters the receiving kettle, a kettle bottom valve of the receiving kettle is opened at the moment after the bath agent is recycled, and the recycled solvent is emptied. And after emptying, continuously raising the temperature of the sublimation kettle, starting to sublimate the 1, 4-naphthoquinone, starting the receiving kettle for stirring at the moment, slowly receiving the sublimated and condensed product 1, 4-naphthoquinone, and finishing purification until the temperature of the sublimation kettle reaches 120 DEG C. The product is not easy to lose in the purification process, and the product is high in yield and environment-friendly. Meanwhile, the recovered solvent can be continuously used for producing a 1, 4-naphthoquinone crude product, so that the cost is saved, and the waste is reduced.

Description

Technical Field

[0001] The utility model relates to the technical field of 1,4-naphthoquinone production, in particular to a 1,4-naphthoquinone purification device. Background Art

[0002] 1,4-Naphthoquinone, yellow crystal, melting point 119-122℃, mainly used in the synthesis of pesticides, fungicides and dye intermediates.

[0003] Currently, 1,4-naphthoquinone is mostly prepared using a liquid-phase oxidation method. The specific steps include: naphthalene as the raw material is dissolved in a solvent, and a liquid-phase oxidation reaction is performed to produce a crude 1,4-naphthoquinone product. The crude 1,4-naphthoquinone is then centrifuged and dried in an oven or a double cone. This drying method has disadvantages such as high product loss, low yield, and poor operating environment. Summary of the Invention

[0004] The technical problem to be solved by the utility model is: in view of the deficiencies in the prior art, a 1,4-naphthoquinone purification device is provided, which has high product yield and is environmentally friendly.

[0005] In order to solve the above technical problems, the technical solution of the utility model is:

[0006] A 1,4-naphthoquinone purification device comprises a 1,4-naphthoquinone solution tank, the outlet of the 1,4-naphthoquinone solution tank is connected to a sublimation kettle via a pipeline, the top outlet of the sublimation kettle is connected to a receiving kettle via a pipeline, and the bottom outlet of the receiving kettle is connected to a solvent receiving tank and a 1,4-naphthoquinone product tank via pipelines respectively.

[0007] As an improved technical solution, the top gas phase outlet of the receiving kettle is connected to a condenser through a pipeline, and the lower outlet of the condenser is connected to a solvent recovery tank through a pipeline.

[0008] As an improved technical solution, the jacket of the receiving kettle is connected to a cooling brine inlet pipe and a cooling brine outlet pipe respectively.

[0009] As an improved technical solution, the jacket of the sublimation kettle is respectively connected to a first steam inlet pipe and a first condensate outlet pipe, the steam inlet pipe is provided with a first automatic regulating valve, the sublimation kettle is provided with a first temperature sensor, and the first automatic regulating valve and the first temperature sensor are interlocked to a control system.

[0010] As an improved technical solution, a heat-insulating jacket is provided on the outside of the pipeline between the sublimation kettle and the receiving kettle.

[0011] As an improved technical solution, the insulation jacket is respectively connected to a second steam inlet pipe and a second condensate outlet pipe, a second temperature sensor is provided on the inlet pipe of the receiving kettle, and a second automatic regulating valve is provided on the second steam inlet pipe. The second automatic regulating valve and the second temperature sensor are interlocked to the control system.

[0012] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:

[0013] The utility model discloses a 1,4-naphthoquinone purification device, comprising a 1,4-naphthoquinone solution tank, the outlet of which is connected to a sublimation kettle via a pipeline, the top outlet of which is connected to a receiving kettle via a pipeline, and the bottom outlet of which is connected to a solvent receiving tank and a 1,4-naphthoquinone product tank via pipelines. A 1,4-naphthoquinone solution is added to the sublimation kettle, which is then slowly heated to 60°C. The solvent evaporates and enters the receiving kettle. When the sublimation kettle temperature reaches 80°C, the bath solvent is recovered. The bottom valve of the receiving kettle is then opened to vent the recovered solvent. After venting, the sublimation kettle temperature is further increased to begin sublimation of the 1,4-naphthoquinone. The receiving kettle is then opened and stirred to slowly receive the sublimated and condensed 1,4-naphthoquinone product until the sublimation kettle temperature reaches 120°C, completing purification. The product purification process is less susceptible to loss, resulting in a high product yield and environmentally friendly performance. Furthermore, the recovered solvent can be reused in the production of crude 1,4-naphthoquinone, saving costs and reducing waste.

[0014] The top gas phase outlet of the receiving kettle of the utility model is connected to a condenser through a pipeline, and the lower outlet of the condenser is connected to a solvent recovery tank through a pipeline, so that the solvent that has not been condensed by the receiving kettle is captured and collected, thereby avoiding direct discharge into the air to cause environmental pollution and reducing the waste of raw materials.

[0015] The jacket of the receiving kettle is respectively connected with a cooling brine water inlet pipe and a cooling brine water outlet pipe, so the cooling speed is fast and the cooling effect on the solvent and the product 1,4-naphthoquinone is good.

[0016] The jacket of the sublimation kettle is connected to a first steam inlet pipe and a first condensate outlet pipe, respectively. A first automatic regulating valve is installed on the steam inlet pipe. A first temperature sensor is located within the sublimation kettle. The first automatic regulating valve and the first temperature sensor are interlocked with a control system. The control system adjusts the opening of the first automatic regulating valve based on the value of the first temperature sensor to maintain the temperature of the sublimation kettle within an appropriate range, facilitating the staged distillation of the solvent and 1,4-naphthoquinone, and improving product purity.

[0017] An insulation jacket is provided on the outside of the pipe between the sublimation kettle and the receiving kettle to prevent condensation of the solvent and 1,4-naphthoquinone on the pipe between the sublimation kettle and the receiving kettle during the distillation process, which would cause material backflow and affect the sublimation efficiency and product purity.

[0018] The insulating jacket is connected to a second steam inlet pipe and a second condensate outlet pipe, respectively. A second temperature sensor is provided on the inlet pipe of the receiving kettle, and a second automatic regulating valve is provided on the second steam inlet pipe. The second automatic regulating valve and the second temperature sensor are interlocked with a control system. The control system adjusts the opening of the second automatic regulating valve based on the value of the second temperature sensor to maintain the temperature of the pipe between the sublimation kettle and the receiving kettle within a suitable range, thereby preventing condensation of material in the pipe and causing backflow. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0020] Figure 1 It is a structural schematic diagram of an embodiment of the utility model;

[0021] Wherein: 1, 4-naphthoquinone solution tank; 2, sublimation kettle; 3, receiving kettle; 4, solvent receiving tank; 5, 1, 4-naphthoquinone product tank; 6, condenser; 7, solvent recovery tank; 8, cooling brine inlet pipe; 9, cooling brine outlet pipe; 10, first steam inlet pipe; 11, first condensate outlet pipe; 12, first automatic regulating valve; 13, first temperature sensor; 14, insulation jacket; 15, second steam inlet pipe; 16, second condensate outlet pipe; 17, second temperature sensor; 18, second automatic regulating valve. DETAILED DESCRIPTION

[0022] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0023] like Figure 1As shown, a 1,4-naphthoquinone purification device includes a 1,4-naphthoquinone solution tank 1. The outlet of the 1,4-naphthoquinone solution tank 1 is connected to a sublimation reactor 2 via a pipeline. The top outlet of the sublimation reactor 2 is connected to a receiving reactor 3 via a pipeline. The bottom outlet of the receiving reactor 3 is connected to a solvent receiving tank 4 and a 1,4-naphthoquinone product tank 5 via pipelines. The 1,4-naphthoquinone solution is added to the sublimation reactor 2, which is then slowly heated to 60°C. The solvent evaporates and enters the receiving reactor 3. When the temperature of the sublimation reactor 2 reaches 80°C, the bath solvent is recovered. The bottom valve of the receiving reactor 3 is opened to vent the recovered solvent. After venting, the temperature of the sublimation reactor 2 is further increased to begin sublimation of the 1,4-naphthoquinone. The receiving reactor 3 is then opened and stirred to slowly receive the sublimated and condensed 1,4-naphthoquinone product until the temperature of the sublimation reactor 2 reaches 120°C, completing the purification process. The product is unlikely to suffer losses during purification, has a high yield, and is environmentally friendly. At the same time, the recovered solvent can be further used in the production of crude 1,4-naphthoquinone, thus saving costs and reducing waste.

[0024] The top gas phase outlet of the receiving kettle 3 is connected to a condenser 6 through a pipeline, and the lower outlet of the condenser 6 is connected to a solvent recovery tank 7 through a pipeline, so as to capture and collect the solvent that has not been condensed by the receiving kettle 3, thereby avoiding direct discharge into the air to cause environmental pollution and reducing the waste of raw materials.

[0025] The jacket of the receiving kettle 3 is connected to a cooling brine inlet pipe 8 and a cooling brine outlet pipe 9 respectively, so the cooling speed is fast and the cooling effect on the solvent and the product 1,4-naphthoquinone in the receiving kettle 3 is good.

[0026] The jacket of the sublimation kettle 2 is connected to a first steam inlet pipe 10 and a first condensate outlet pipe 11, respectively. A first automatic regulating valve 12 is installed on the steam inlet pipe. A first temperature sensor 13 is located within the sublimation kettle 2. The first automatic regulating valve 12 and the first temperature sensor 13 are interlocked with a control system. The control system adjusts the opening of the first automatic regulating valve 12 based on the value of the first temperature sensor 13 to maintain the temperature of the sublimation kettle 2 within an appropriate range, facilitating the staged distillation of the solvent and 1,4-naphthoquinone and improving product purity.

[0027] An insulating jacket 14 is provided on the outside of the pipe between the sublimation kettle 2 and the receiving kettle 3 to prevent condensation of the solvent and 1,4-naphthoquinone on the pipe between the sublimation kettle 2 and the receiving kettle 3 during the distillation process, which may cause material reflux and affect the sublimation efficiency and product purity.

[0028] The insulating jacket 14 is connected to a second steam inlet pipe 15 and a second condensate outlet pipe 16, respectively. A second temperature sensor 17 is provided on the inlet pipe of the receiving kettle 3. A second automatic regulating valve 18 is also provided on the second steam inlet pipe 15. The second automatic regulating valve 18 and the second temperature sensor 17 are interlocked with the control system. The control system adjusts the opening of the second automatic regulating valve 18 based on the value of the second temperature sensor 17 to maintain the temperature of the pipe between the sublimation kettle 2 and the receiving kettle 3 within a suitable range, thereby preventing condensation of material within the pipe and causing backflow.

[0029] It should be understood that these embodiments are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the contents of the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.

Claims

1. A 1,4-naphthoquinone purification device, comprising a 1,4-naphthoquinone solution tank, characterized in that: The outlet of the 1,4-naphthoquinone solution tank is connected to a sublimation kettle through a pipeline, the top outlet of the sublimation kettle is connected to a receiving kettle through a pipeline, and the bottom outlet of the receiving kettle is connected to a solvent receiving tank and a 1,4-naphthoquinone product tank through pipelines respectively.

2. A 1,4-naphthoquinone purification device according to claim 1, characterized in that: The top gas phase outlet of the receiving kettle is connected to a condenser through a pipeline, and the lower outlet of the condenser is connected to a solvent recovery tank through a pipeline.

3. The 1,4-naphthoquinone purification device according to claim 1, characterized in that: The jacket of the receiving kettle is respectively connected with a cooling brine water inlet pipe and a cooling brine water outlet pipe.

4. The 1,4-naphthoquinone purification device according to claim 1, characterized in that: The jacket of the sublimation kettle is respectively connected to a first steam inlet pipe and a first condensate outlet pipe, the steam inlet pipe is provided with a first automatic regulating valve, the sublimation kettle is provided with a first temperature sensor, and the first automatic regulating valve and the first temperature sensor are interlocked to a control system.

5. The 1,4-naphthoquinone purification device according to claim 1, characterized in that: A heat-insulating jacket is provided on the outside of the pipeline between the sublimation kettle and the receiving kettle.

6. A 1,4-naphthoquinone purification device according to claim 5, characterized in that: The thermal insulation jacket is respectively connected to a second steam inlet pipe and a second condensate outlet pipe. A second temperature sensor is provided on the inlet pipe of the receiving kettle. A second automatic regulating valve is provided on the second steam inlet pipe. The second automatic regulating valve and the second temperature sensor are interlocked to a control system.

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