Continuous acidification device for 1, 3-cyclohexanedione

Abstract

The utility model discloses a continuous acidification device for 1, 3-cyclohexanedione, which relates to the technical field of acidification devices, and comprises a first acidification kettle, a second acidification kettle and a solid-liquid separation module, the first acidification kettle is used for storing reaction raw materials, and is provided with a hydrogenated liquid adding port and a first acid liquid adding port; a solution outlet of the first acidification kettle is connected with a solution inlet of the second acidification kettle through an overflow pipeline, the second acidification kettle is further provided with a second acid liquor adding port, a solution outlet of the second acidification kettle is connected with a solution inlet of the solid-liquid separation module through a pipeline, and the solid-liquid separation module comprises a plurality of centrifugal separation units which are sequentially communicated. And a leacheate adding opening is formed in one centrifugal separation unit. According to the utility model, continuous acidification reaction can be realized, and the production efficiency is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of acid precipitation devices, in particular to a continuous acid precipitation device for 1,3 - cyclohexanedione. Background Art

[0002] The acid precipitation production process of 1,3 - cyclohexanedione is as follows: after dissolving raw material resorcinol in liquid alkali, a hydrogenated solution is obtained through hydrogenation, and the hydrogenated solution is acidified by dropping hydrochloric acid to obtain 1,3 - cyclohexanedione.

[0003] However, at present, each process flow is an intermittent reaction, resulting in a long reaction time, low efficiency, and large equipment and floor area required. Summary of the Utility Model

[0004] The purpose of the utility model is to provide a continuous acid precipitation device for 1,3 - cyclohexanedione to solve the problems existing in the above - mentioned prior art, realize continuous acid precipitation reaction, and improve production efficiency.

[0005] To achieve the above - mentioned purpose, the utility model provides the following scheme:

[0006] The utility model provides a continuous acid precipitation device for 1,3 - cyclohexanedione, which includes a first acid precipitation kettle, a second acid precipitation kettle and a solid - liquid separation module. The first acid precipitation kettle is used to store reaction raw materials, and a hydrogenated solution inlet and a first acid solution inlet are arranged on the first acid precipitation kettle. The solution outlet of the first acid precipitation kettle is connected to the solution inlet of the second acid precipitation kettle through an overflow pipeline. A second acid solution inlet is also arranged on the second acid precipitation kettle. The solution outlet of the second acid precipitation kettle is connected to the solution inlet of the solid - liquid separation module through a pipeline. The solid - liquid separation module includes a plurality of centrifugal separation units connected in sequence, and a washing liquid inlet is arranged on one of the centrifugal separation units.

[0007] Preferably, a first temperature control element is also arranged on the first acid precipitation kettle, and the first temperature control element is used to control the temperature in the first acid precipitation kettle between 20°C and 25°C.

[0008] Preferably, the first acid solution inlet is used to add hydrochloric acid into the first acid precipitation kettle and make the pH in the first acid precipitation kettle between 2 and 3. A first stirring element is also arranged in the first acid precipitation kettle, and the first stirring element is used to stir the solution in the first acid precipitation kettle.

[0009] Preferably, the hydrogenated solution inlet is used to add hydrogenated solution into the first acid precipitation kettle.

[0010] Preferably, a first pH meter and a first thermometer are installed on the first acid precipitation kettle, and the detection ends of the first pH meter and the first thermometer both extend into the interior of the first acid precipitation kettle; a second pH meter and a second thermometer are installed on the second acid precipitation kettle, and the detection ends of the second pH meter and the second thermometer both extend into the interior of the second acid precipitation kettle.

[0011] Preferably, valves are provided at the hydrogenated liquid inlet, the first acid liquid inlet, the second acid liquid inlet, and each solution outlet, and the first pH meter, the first thermometer, the second pH meter, the second thermometer, and each valve are electrically connected to a controller.

[0012] Preferably, a second temperature control element is further provided on the second acid precipitation kettle, and the second temperature control element is used to control the temperature in the second acid precipitation kettle to be between 10°C and 20°C.

[0013] Preferably, the second acid liquid inlet is used to add hydrochloric acid into the second acid precipitation kettle to make the pH in the second acid precipitation kettle between 1 and 2; a second stirring element is further provided in the second acid precipitation kettle, and the second stirring element is used to stir the solution in the second acid precipitation kettle.

[0014] Preferably, a buffer tank is provided between the solution outlet of the second acid precipitation kettle and the solution inlet of the solid-liquid separation module.

[0015] Preferably, there are three centrifugal separation units, namely a first centrifugal separation unit, a second centrifugal separation unit, and a third centrifugal separation unit. Centrifugal liquid outlets for discharging mother liquor are provided on the inner side walls of both the first centrifugal separation unit and the third centrifugal separation unit, a washing liquid inlet is provided on the side wall of the second centrifugal separation unit, and conveying elements are provided in each of the first centrifugal separation unit, the second centrifugal separation unit, and the third centrifugal separation unit.

[0016] The present utility model has achieved the following technical effects compared with the prior art:

[0017] The continuous acid precipitation device for 1,3 - cyclohexanedione provided by the present utility model has a first acid precipitation kettle for storing reaction raw materials, and through processes such as acid precipitation on the reaction raw materials, the required 1,3 - cyclohexanedione is produced. The first acid precipitation kettle is provided with a hydrogenated liquid inlet and a first acid liquid inlet. The hydrogenated liquid is added into the first acid precipitation kettle through the hydrogenated liquid inlet, and hydrochloric acid is added into the first acid precipitation kettle through the first acid liquid inlet. The first acid precipitation kettle is used as a mixing storage tank, and then the hydrogenated liquid is acidified with hydrochloric acid and cooled for crystallization. The solution outlet of the first acid precipitation kettle is connected to the solution inlet of the second acid precipitation kettle through an overflow pipeline, so as to overflow the mixed liquid in the first acid precipitation kettle into the second acid precipitation kettle. The second acid precipitation kettle is also provided with a second acid liquid inlet, and then hydrochloric acid is added into the second acid precipitation kettle to enable the mixed liquid to react again in the second acid precipitation kettle, generating 1,3 - cyclohexanedione doped with mother liquor. The solution outlet of the second acid precipitation kettle is connected to the solution inlet of the solid - liquid separation module through a pipeline to introduce the 1,3 - cyclohexanedione doped with mother liquor into the solid - liquid separation module for separation. The solid - liquid separation module includes a plurality of sequentially connected centrifugal separation units, and through centrifugal action, the mother liquor is thrown out. And a washing liquid inlet is provided on one of the centrifugal separation units. Since sodium chloride is generated when the hydrogenated liquid reacts with hydrochloric acid, the sodium chloride on the surface of 1,3 - cyclohexanedione is washed with the washing liquid to ensure the quality of 1,3 - cyclohexanedione. At the same time, through the design of the above components, the continuous production of 1,3 - cyclohexanedione is realized, and the production efficiency is improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions in the embodiments of the present utility model or the prior art, the following will briefly introduce the drawings required to be used in the embodiments. Obviously, the drawings described below are only some embodiments of the present utility model. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0019] Figure 1 It is a schematic structural diagram of the continuous acid precipitation device for 1,3 - cyclohexanedione in the present utility model;

[0020] Figure 2 It is a schematic structural diagram of the first acid precipitation kettle in the present utility model;

[0021] Figure 3 It is a schematic structural diagram of the second acid precipitation kettle in the present utility model;

[0022] Figure 4 It is a schematic structural diagram of the solid - liquid separation module in the present utility model;

[0023] In the figure: 1 - first acid precipitation kettle, 2 - second acid precipitation kettle, 3 - solid-liquid separation module, 4 - buffer tank, 5 - valve, 6 - hydrogenated liquid inlet, 7 - first acid liquid inlet, 8 - first stirring element, 9 - first pH meter, 10 - first thermometer, 11 - overflow outlet, 12 - overflow inlet, 13 - second acid liquid inlet, 14 - second stirring element, 15 - second pH meter, 16 - second thermometer, 17 - first centrifugal separation unit, 18 - second centrifugal separation unit, 19 - third centrifugal separation unit, 20 - conveying element. Detailed implementation manners

[0024] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0025] The object of the present invention is to provide a continuous acid precipitation device for 1,3 - cyclohexanedione to solve the problems existing in the prior art, realize continuous acid precipitation reaction, and improve production efficiency.

[0026] To make the above objects, features, and advantages of the present invention more obvious and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific implementation manners.

[0027] As Figures 1-4As shown in the figure, this embodiment provides a continuous acid precipitation device for 1,3-cyclohexanedione, which includes a first acid precipitation kettle 1, a second acid precipitation kettle 2 and a solid-liquid separation module 3. The first acid precipitation kettle 1 is used to store reaction raw materials, and through processes such as acid precipitation of the reaction raw materials, the required 1,3-cyclohexanedione is produced. A hydrogenated liquid inlet 6 and a first acid liquid inlet 7 are provided on the first acid precipitation kettle 1. The hydrogenated liquid is added into the first acid precipitation kettle 1 through the hydrogenated liquid inlet 6, and hydrochloric acid is added into the first acid precipitation kettle 1 through the first acid liquid inlet 7. The first acid precipitation kettle 1 is used as a mixing storage tank, and then the hydrogenated liquid is acidified with hydrochloric acid and cooled for crystallization. The solution outlet (i.e., the overflow outlet 11) of the first acid precipitation kettle 1 is connected to the solution inlet (i.e., the overflow inlet 12) of the second acid precipitation kettle 2 through an overflow pipe, so as to overflow the mixed liquid in the first acid precipitation kettle 1 into the second acid precipitation kettle 2. A second acid liquid inlet 13 is also provided on the second acid precipitation kettle 2, and then hydrochloric acid is added into the second acid precipitation kettle 2 to make the mixed liquid react again in the second acid precipitation kettle 2 to generate 1,3-cyclohexanedione doped with mother liquor. The solution outlet of the second acid precipitation kettle 2 is connected to the solution inlet of the solid-liquid separation module 3 through a pipe to introduce the 1,3-cyclohexanedione doped with mother liquor into the solid-liquid separation module 3 for separation. The solid-liquid separation module 3 includes a plurality of sequentially connected centrifugal separation units. Through centrifugal action, the mother liquor is thrown out, and a washing liquid inlet is provided on one of the centrifugal separation units. Since sodium chloride is generated when the hydrogenated liquid reacts with hydrochloric acid, the sodium chloride on the surface of 1,3-cyclohexanedione is washed with the washing liquid to ensure the quality of 1,3-cyclohexanedione. At the same time, through the design of the above components, a continuous acid precipitation process and a continuous centrifugal discharging process are realized, thereby realizing the continuous production of 1,3-cyclohexanedione, reducing manual operation, reducing intermediate processes, and improving production efficiency.

[0028] Specifically, a first temperature control element is further provided on the first acid precipitation kettle 1. The first temperature control element can be a jacket, etc. The first temperature control element is used to control the temperature in the first acid precipitation kettle 1 between 20°C and 25°C to meet the reaction requirements.

[0029] The first acid liquid inlet 7 is used to add hydrochloric acid into the first acid precipitation kettle 1 and make the pH in the first acid precipitation kettle 1 between 2 and 3 to reach the required pH value for the reaction. A first stirring element 8 is also provided in the first acid precipitation kettle 1. The first stirring element 8 is used to stir the solution in the first acid precipitation kettle 1 to improve the mixing uniformity and thus improve the reaction efficiency.

[0030] The hydrogenated liquid inlet 6 is used to add hydrogenated liquid into the first acid precipitation kettle 1.

[0031] A first acid precipitation kettle 1 is equipped with a first pH meter 9 and a first thermometer 10. The detection ends of the first pH meter 9 and the first thermometer 10 both extend into the interior of the first acid precipitation kettle 1, thereby enabling real-time monitoring of the pH value and temperature inside the first acid precipitation kettle 1, so as to know the reaction situation. A second acid precipitation kettle 2 is equipped with a second pH meter 15 and a second thermometer 16. The detection ends of the second pH meter 15 and the second thermometer 16 both extend into the interior of the second acid precipitation kettle 2, thereby enabling real-time monitoring of the pH value and temperature inside the first acid precipitation kettle 1, so as to know the reaction situation.

[0032] The second acid precipitation kettle 2 is also provided with a second temperature control element, and the second temperature control element is used to control the temperature inside the second acid precipitation kettle 2 to be between 10°C and 20°C.

[0033] Valves 5 are provided at the hydrogenated liquid inlet 6, the first acid liquid inlet 7, the second acid liquid inlet 13, and each solution outlet. The first pH meter 9, the first thermometer 10, the second pH meter 15, the second thermometer 16, and each valve 5 are all electrically connected to a controller. Then, according to the actual pH value and temperature value, the opening and closing of the corresponding valve 5 and the temperature control element are automatically controlled by the controller. Through automatic control, quantitative dropping is achieved, and the pH range is accurately controlled. For example, when the first pH meter 9 or the second pH meter 15 detects that the pH inside the corresponding first acid precipitation kettle 1 or the second acid precipitation kettle 2 is too high, the opening of the corresponding valve 5 is electrically controlled by the controller to adjust the amount of hydrochloric acid introduced.

[0034] The second acid liquid inlet 13 is used to add hydrochloric acid into the second acid precipitation kettle 2 and make the pH inside the second acid precipitation kettle 2 between 1 and 2. A second stirring element 14 is also provided inside the second acid precipitation kettle 2, and the second stirring element 14 is used to stir the solution inside the second acid precipitation kettle 2 to improve the mixing uniformity, reaction efficiency, and reaction effect.

[0035] A buffer tank 4 is provided between the solution outlet of the second acid precipitation kettle 2 and the solution inlet of the solid-liquid separation module 3. The buffer tank 4 serves to temporarily store the overflow solution.

[0036] There are three centrifugal separation units, namely the first centrifugal separation unit 17, the second centrifugal separation unit 18, and the third centrifugal separation unit 19. Centrifugal liquid discharge ports for discharging the mother liquor are provided on the inner side walls of both the first centrifugal separation unit 17 and the third centrifugal separation unit 19. A washing liquid inlet is provided on the side wall of the second centrifugal separation unit 18, and the washing liquid inlet can be used to add chilled water. Under the action of centrifugal force, the mother liquor and 1,3-cyclohexanedione are preliminarily separated by the first centrifugal separation unit 17, and then the separated 1,3-cyclohexanedione is introduced into the second centrifugal separation unit 18 and washed in the second centrifugal separation unit 18 to wash away sodium chloride. The washed 1,3-cyclohexanedione is introduced into the third centrifugal separation unit 19, and then continues to be centrifugally separated in the third centrifugal separation unit 19 to discharge the mother liquor and chilled water, etc. Finally, the remaining is qualified 1,3-cyclohexanedione. Conveying elements 20 are provided in the first centrifugal separation unit 17, the second centrifugal separation unit 18, and the third centrifugal separation unit 19 to achieve the conveyance and export of materials. At the same time, through the setting of the centrifugal separation units, continuous feeding and continuous discharging can be achieved, improving production efficiency. At the same time, it ensures that the impurity content of the final wet product meets the standards.

[0037] The working process of this embodiment is as follows:

[0038] First, hydrochloric acid is added in advance to the first acid precipitation kettle 1, and stirring is performed by the first stirring element 8, controlling the temperature to be 20°C - 25°C. Then, the hydrogenated liquid and hydrochloric acid are simultaneously dropped into the first acid precipitation kettle 1, and stirring continues, and the temperature is continuously controlled to be 20°C - 25°C, and the pH is controlled to be between 2 and 3. When the height of the solution in the first acid precipitation kettle 1 reaches the overflow outlet 11, it overflows to the second acid precipitation kettle 2 through the overflow outlet 11 on the first acid precipitation kettle 1;

[0039] Then, hydrochloric acid is dropped into the second acid precipitation kettle 2, controlling the pH of the solution in the second acid precipitation kettle 2 to be between 1 and 2, and controlling the temperature to be between 10°C and 20°C. Then, the solution is stirred by the second stirring element 14 to keep the pH of the solution in the second acid precipitation kettle 2 between 1 and 2. Then, it is discharged by overflow to the buffer tank 4 and continuously cooled to 5°C;

[0040] Finally, the suspension in the buffer tank 4 is subjected to multi-stage separation by the solid-liquid separation module 3 to obtain the wet product of solid 1,3-cyclohexanedione.

[0041] Specific examples are applied in the present utility model to elaborate on the principle and implementation manner of the present utility model. The descriptions of the above embodiments are only used to help understand the method and its core idea of the present utility model; at the same time, for those of ordinary skill in the art, according to the idea of the present utility model, there will be changes in the specific implementation manner and application scope. In summary, the content of this specification should not be construed as a limitation on the present utility model.

Claims

1. A continuous acid precipitation device for 1,3 - cyclohexanedione, characterized in that: It includes a first acid precipitation kettle, a second acid precipitation kettle and a solid-liquid separation module. The first acid precipitation kettle is used to store reaction raw materials, and a hydrogenated liquid inlet and a first acid liquid inlet are provided on the first acid precipitation kettle. The solution outlet of the first acid precipitation kettle is connected to the solution inlet of the second acid precipitation kettle through an overflow pipeline. A second acid liquid inlet is also provided on the second acid precipitation kettle. The solution outlet of the second acid precipitation kettle is connected to the solution inlet of the solid-liquid separation module through a pipeline. The solid-liquid separation module includes a plurality of centrifugal separation units connected in sequence, and a washing liquid inlet is provided on one of the centrifugal separation units.

2. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: A first temperature control element is also provided on the first acid precipitation kettle, and the first temperature control element is used to control the temperature in the first acid precipitation kettle to be between 20°C and 25°C.

3. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: The first acid liquid inlet is used to add hydrochloric acid into the first acid precipitation kettle and make the pH in the first acid precipitation kettle between 2 and 3. A first stirring element is also provided in the first acid precipitation kettle, and the first stirring element is used to stir the solution in the first acid precipitation kettle.

4. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: The hydrogenated liquid inlet is used to add hydrogenated liquid into the first acid precipitation kettle.

5. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: A first pH meter and a first thermometer are installed on the first acid precipitation kettle, and the detection ends of the first pH meter and the first thermometer both extend into the interior of the first acid precipitation kettle. A second pH meter and a second thermometer are installed on the second acid precipitation kettle, and the detection ends of the second pH meter and the second thermometer both extend into the interior of the second acid precipitation kettle.

6. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 5, wherein: Valves are provided at the hydrogenated liquid inlet, the first acid liquid inlet, the second acid liquid inlet and each solution outlet. The first pH meter, the first thermometer, the second pH meter, the second thermometer and each valve are all electrically connected to a controller.

7. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: A second temperature control element is also provided on the second acid precipitation kettle, and the second temperature control element is used to control the temperature in the second acid precipitation kettle to be between 10°C and 20°C.

8. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: The second acid liquid inlet is used to add hydrochloric acid into the second acid precipitation kettle and make the pH in the second acid precipitation kettle between 1 and 2. A second stirring element is also provided in the second acid precipitation kettle, and the second stirring element is used to stir the solution in the second acid precipitation kettle.

9. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: A buffer tank is provided between the solution outlet of the second acid precipitation kettle and the solution inlet of the solid-liquid separation module.

10. The continuous acid precipitation device for 1,3 - cyclohexanedione according to claim 1, characterized in that: There are three centrifugal separation units, which are the first centrifugal separation unit, the second centrifugal separation unit and the third centrifugal separation unit respectively. Centrifugal liquid outlets for discharging mother liquid are provided on the inner side walls of both the first centrifugal separation unit and the third centrifugal separation unit. The washing liquid inlet is provided on the side wall of the second centrifugal separation unit, and conveying elements are provided in the first centrifugal separation unit, the second centrifugal separation unit and the third centrifugal separation unit.

Images