Working solution regeneration and purification system for automatic operation of hydrogen peroxide production

Abstract

The utility model discloses an automatic operating working solution regeneration and purification system for hydrogen peroxide production, which relates to the technical field of hydrogen peroxide production and comprises a working solution regeneration reactor, a first working solution circulating pump, a second working solution circulating pump, a working solution filter, a first working solution coalescer, a second working solution coalescer and a pipeline static mixer. The beneficial effects are that highly automatic operation is realized; compared with the traditional process for regenerating hydrogen peroxide by using alkali liquor in a preparation kettle, due to no intermittent operation stirrer of the preparation kettle, the automatic operation degree is higher, and the failure rate of equipment is lower.

Description

Technical Field

[0001] This utility model relates to the field of hydrogen peroxide production technology, and more specifically, to a working fluid regeneration and purification system for automated operation of hydrogen peroxide production. Background Technology

[0002] The working fluid purification (alkaline washing) process is an auxiliary process for the hydrogen peroxide unit. Its function is as follows: After the hydrogen peroxide unit has been running for a period of time, anthraquinones in the working fluid will degrade to anthrone, hydroxyanthraquinone, hexahydroanthraquinone, octahydroanthraquinone, and other degradation products during the hydrogenation process, and will generate epoxy degradation products during the oxidation process. Most of these degradation products can be reduced to anthraquinone by the action of activated alumina, but some degradation products (such as water-soluble degradation products) cannot be regenerated into anthraquinone by the action of activated alumina and remain in the working fluid. When the amount of degradation products in the working fluid reaches a certain level, the viscosity of the working fluid will increase. When the viscosity of the working fluid increases to a certain level, it will affect the separation time of the working fluid and water in the extraction tower, resulting in material accumulation in the extraction tower, and may even cause water flooding in the extraction zone, affecting the extraction of hydrogen peroxide in the extraction tower. Therefore, this working fluid needs to be regenerated and purified.

[0003] Currently, the main method of regeneration and purification is alkaline washing and purification regeneration. The purpose of alkaline washing and regeneration is to regenerate some of the degradation products and remove some of the degradation products (water-soluble degradation products) by dissolving them in the alkaline solution. The traditional alkaline washing and purification regeneration process sends the working solution (from underground tanks, clay beds, or hydrogenated clay beds) to the preparation vessel for washing. This involves alkali preparation and alkali extraction. Because the alkaline washing working solution in domestic hydrogen peroxide equipment manufacturers is currently operated intermittently (intermittent operation of the preparation vessel makes high automation difficult), operators spend a long time at the preparation unit, increasing their workload, the risk to them, and the risk of human error (most explosions in the preparation process are caused by human error).

[0004] No effective solutions have yet been proposed to address the problems in the relevant technologies. Utility Model Content

[0005] In view of the problems in related technologies, the purpose of this utility model is to propose a working fluid regeneration and purification system for automated operation of hydrogen peroxide production, so as to overcome the above-mentioned technical problems existing in the existing related technologies.

[0006] The technical solution of this utility model is implemented as follows:

[0007] A working fluid regeneration and purification system for automated hydrogen peroxide production includes: a working fluid regeneration reactor, a first working fluid circulation pump, a second working fluid circulation pump, a working fluid filter, a first working fluid coalescer, a second working fluid coalescer, and a pipeline static mixer, wherein;

[0008] The output of the working fluid regeneration reactor is connected to the input of the first working fluid circulation pump and the second working fluid circulation pump, respectively. The outputs of the first working fluid circulation pump and the second working fluid circulation pump are connected to the input of the pipeline static mixer and the input of the working fluid filter, respectively. The output of the working fluid filter is connected to the input of the first working fluid coalescer and the second working fluid coalescer, respectively. The first working fluid coalescer and the second working fluid coalescer are connected in parallel. The outputs of the first working fluid coalescer, the second working fluid coalescer, and the pipeline static mixer are connected in parallel to the input of the working fluid regeneration reactor, respectively.

[0009] Furthermore, the output end of the working fluid regeneration reactor 1 is also connected to an alkali metering tank and a phosphoric acid metering tank, and the alkali metering tank and the phosphoric acid metering tank are respectively connected to the input ends of the first working fluid circulation pump and the second working fluid circulation pump.

[0010] Furthermore, the alkali metering tank and the phosphoric acid metering tank are respectively connected to the first working fluid circulation pump and the second working fluid circulation pump through the eighth valve and the ninth valve.

[0011] Furthermore, the pipeline static mixer is connected to the first working fluid circulation pump via a first valve, and the pipeline static mixer is connected to the working fluid filter via a second valve.

[0012] Furthermore, the first working fluid coalescer is connected to the working fluid filter via a third valve, and the second working fluid coalescer is connected to the working fluid filter via a fourth valve.

[0013] Furthermore, the pipeline static mixer is connected to the working fluid regeneration reactor via a fifth valve.

[0014] Furthermore, the first working fluid coalescer and the second working fluid coalescer are connected to the working fluid regeneration reactor via the sixth valve and the seventh valve, respectively.

[0015] The beneficial effects of this utility model are:

[0016] 1. This alkaline washing and regeneration purification system is suitable for green and efficient all-acid hydrogen peroxide production equipment or for converting traditional acid-base hydrogen peroxide production processes into green and efficient all-acid hydrogen peroxide production processes. Since this new alkaline washing and regeneration purification system processes approximately 10 to 20 cubic meters of working liquid per day, it is well-suited for green and efficient all-acid hydrogen peroxide production equipment (hydrogen peroxide production processes that produce less degradation products).

[0017] 2. Enhanced safety: The addition of a hydrogen peroxide content analyzer and a pH analyzer to the utility model allows for direct monitoring of the hydrogen peroxide content and pH value in the working solution during alkali addition. This prevents accidents such as decomposition and explosion caused by the direct addition of alkali to the working solution with excessive hydrogen peroxide content, as is common in traditional alkali washing and regeneration systems.

[0018] 3. Compared to traditional preparation kettles, the alkali washing and regeneration purification effect is better, mainly due to the more thorough mixing of alkali and working solution. Firstly, it features a two-stage mixing system: a pipeline mixer and a large mixing reactor. Secondly, once alkali settles at the bottom of the regeneration reactor, it is immediately pumped to the pipeline mixer by the working solution circulation pump to mix with the working solution, fully utilizing the regeneration effect of the alkali. In contrast, in traditional preparation kettles, if some alkali enters, it easily settles at the bottom (the agitator is unlikely to stir up the settled alkali at the bottom and mix it with the working solution), failing to achieve the desired alkali washing and regeneration effect, resulting in low alkali utilization.

[0019] 4. Compared with traditional processes, the alkali solution and working solution are easier to separate. The working solution after washing and regenerating the alkali solution is darker in color and not much different from the color of the alkali solution used for washing. When the alkali solution is left to stand at the bottom of the preparation vessel for discharge, it is difficult to distinguish the interface between the working solution and the alkali solution with the naked eye, which easily leads to the working solution being discharged into the working solution recovery tank. However, the working solution after washing and regenerating the alkali solution has a larger density difference from the alkali solution used for washing, and it is easier to separate in the working solution coalescing tank. It can be easily discharged into the working solution recovery tank through the interface gauge control valve.

[0020] 5. This utility model can achieve a high degree of automated operation; compared with the traditional process of regenerating hydrogen peroxide from alkaline solution in the preparation tank, since there is no intermittently running agitator in the preparation tank, the degree of automation is higher and the equipment failure rate is lower.

[0021] Other features and advantages of this invention will be set forth in the description which follows, and will be apparent in part from the description, or may be learned by practicing the invention. The objectives and other advantages of this invention are realized and obtained through the structures particularly pointed out in the description and the accompanying drawings.

[0022] To make the above-mentioned objectives, features and advantages of this utility model more apparent and understandable, preferred embodiments are described below in detail with reference to the accompanying drawings. Attached Figure Description

[0023] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0024] Figure 1 This is a schematic diagram of the working fluid regeneration and purification system for automated operation of hydrogen peroxide production according to an embodiment of the present invention.

[0025] In the picture:

[0026] 1. Working fluid regeneration reactor; 2. First working fluid circulation pump; 3. Second working fluid circulation pump; 4. Working fluid filter; 5. First working fluid coalescer; 6. Second working fluid coalescer; 7. Pipeline static mixer; 8. Alkali metering tank; 9. Phosphoric acid metering tank;

[0027] 10. Tenth valve; 11. First valve; 12. Second valve; 13. Third valve; 14. Fourth valve; 15. Fifth valve; 16. Sixth valve; 17. Seventh valve; 18. Eighth valve; 19. Ninth valve; 20. Eleventh valve. Detailed Implementation

[0028] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present utility model are within the protection scope of the present utility model.

[0029] According to an embodiment of the present invention, a working fluid regeneration and purification system for automated operation of hydrogen peroxide production is provided.

[0030] like Figure 1 As shown, an automated working fluid regeneration and purification system for hydrogen peroxide production includes: a working fluid regeneration reactor 1, a first working fluid circulation pump 2, a second working fluid circulation pump 3, a working fluid filter 4, a first working fluid coalescer 5, a second working fluid coalescer 6, a pipeline static mixer 7, an alkali metering tank 8, and a phosphoric acid metering tank 9, wherein;

[0031] The output end of the working fluid regeneration reactor 1 is connected to the input ends of the first working fluid circulation pump 2 and the second working fluid circulation pump 3, respectively. The output ends of the first working fluid circulation pump 2 and the second working fluid circulation pump 3 are connected to the input ends of the pipeline static mixer 7 and the working fluid filter 4, respectively. The output end of the working fluid filter 4 is connected to the input ends of the first working fluid coalescer 5 and the second working fluid coalescer 6, respectively. The first working fluid coalescer 5 and the second working fluid coalescer 6 are connected in parallel. The output ends of the first working fluid coalescer 5 and the second working fluid coalescer 6, respectively, and the output end of the pipeline static mixer 7 are connected in parallel to the input end of the working fluid regeneration reactor 1.

[0032] With the above-mentioned scheme, the top of the working fluid regeneration reactor 1 has an inlet for externally supplied washing and purification working fluid, an inlet for circulating working fluid, an inlet for heating working fluid vapor, a condensate outlet, and a generated exhaust gas outlet. In addition, there are instrument thermometer interfaces and remote liquid level gauge interfaces. Inside the working fluid regeneration reactor 1, there is a stirring and mixing mechanism and a heater that rely on the pressure of the working fluid inlet.

[0033] A drain sight glass and camera are installed on the pipeline connecting the outlet of the working fluid regeneration reactor 1 to the inlet of the first working fluid circulation pump 2 and the second working fluid circulation pump 3. Below the sight glass is an acidic wastewater discharge pipe and a quick-opening valve. When the working fluid requiring regeneration and purification enters the working fluid regeneration reactor 1, manual observation through the sight glass is required to drain the acidic water inside the sedimentation equipment and some of the dirtier working fluid deposited at the bottom of the working fluid regeneration reactor 1. Simultaneously, the outlet of the working fluid regeneration reactor 1 is also connected to the inlet pipes of the first working fluid circulation pump 2 and the second working fluid circulation pump 3, which are also connected to the alkali metering tank 8 and the phosphoric acid metering tank 9. When the working fluid circulation reaches the alkali washing and regeneration conditions, the alkali solution can be sent to the inlet of the first working fluid circulation pump 2 and the second working fluid circulation pump 3 through the alkali inlet pipe to mix with the working fluid. Then, through the thorough mixing action of the static mixer 7 in the pipeline, the alkali solution reacts with the degradation products in the working fluid in the working fluid regeneration reactor 1, thereby achieving the purpose of regenerating the degradation products.

[0034] The purpose of adding a pure water pipeline to the alkali solution pipeline is to dilute the alkali in the working solution after alkali washing with pure water before removing it through the first working solution coalescer 5. The purpose of adding a phosphoric acid pipeline is to add a certain amount of phosphoric acid to the water-washed working solution to adjust its pH to weakly acidic, providing a safety guarantee for entering the fully acidic hydrogen peroxide unit. The working solution enters through the inlet of the first working solution coalescer 5. After passing through the first working solution coalescer 5, the free alkali in it is coalesced into large alkali droplets and deposited at the bottom of the coalescer. When a certain amount of water has settled at the bottom of the first working solution coalescer 5, the alkaline water is discharged to the alkaline side of the working solution recovery tank.

[0035] The parallel analyzer of the pipeline static mixer 7 mainly analyzes and detects the hydrogen peroxide content and pH value of the working fluid. When the hydrogen peroxide content of the delivered material is found to be high, it cannot be directly regenerated and purified by adding alkali solution. The hydrogen peroxide content in the working fluid needs to be reduced to below 0.15 g / L before adding alkali solution for washing and regeneration. After washing, regeneration and purification, the working fluid needs to be adjusted to pH value and then passed through the second working fluid coalescer 6 to remove acidic water before it can be sent to the hydrogen peroxide dilution unit for use. If the pH value is too high, it will cause hydrogen peroxide decomposition, which poses a certain risk to the main unit.

[0036] This technical solution specifically includes the following steps:

[0037] When the liquid level in the working fluid regeneration reactor 1 reaches 70% to 90%, an alarm is triggered, and the automatic heating of the working fluid is activated, with the temperature set at 50℃. The second valve 12, the fourth valve 14, and the sixth valve 16 need to be opened, and the first working fluid circulation pump 2 and the second working fluid circulation pump 3 are started. Water is drained through the first working fluid coalescer 6. When the water is drained and the liquid level in the working fluid regeneration reactor 1 is less than 70%, the second valve 12, the fourth valve 14, and the sixth valve 16 are closed, and the first working fluid circulation pump 2 and the second working fluid circulation pump 3 are stopped to continue waiting for feed.

[0038] When the liquid level is still between 70% and 90% after draining the water, confirm to turn on the automatic regeneration and purification washing button; start program one;

[0039] Procedure 1: Open the first valve 11 and the fifth valve 15, and close the second valve 12, the fourth valve 14, the sixth valve 16, the first working fluid circulation pump 2, and the second working fluid circulation pump 3.

[0040] Procedure 2: After running for 20 minutes, detect the hydrogen peroxide content in the working solution. If the detected hydrogen peroxide content is greater than 0.15 g / L, proceed to Procedure 3. If the detected hydrogen peroxide content is less than or equal to 0.15 g / L, proceed to Procedure 5.

[0041] Procedure 3: Open valve 10 and add 1m of pure water using a flow meter. 3 Then close valve 10 and run for 40 minutes. Run procedure four.

[0042] Procedure 4: If the hydrogen peroxide content is less than or equal to 0.15 g / L, open valves 12, 14, and 16, and close valves 11 and 15. Run the process for 30 minutes. The water will be automatically discharged to the acidic side of the working liquid recovery tank via the second working liquid coalescer 6. Then, open valves 11 and 15, and close valves 12, 14, and 16 to run Procedure 5. If the hydrogen peroxide content is greater than 0.15 g / L, run Procedure 3.

[0043] Procedure 5: Open valve 8 and use the level gauge in alkali metering tank 8 to deliver 300L of alkali solution with a concentration of 10% to the inlet of the first working fluid circulation pump 2 for mixing and regeneration with the working fluid. After closing valve 8, run the device for 60 minutes; then proceed to procedure 6.

[0044] Procedure Six: Open valves 12, 13, and 16; close valves 11 and 15. Run for 30 minutes, allowing the alkaline droplets mixed in the working fluid to settle at the bottom as they pass through the first working fluid coalescer 5. Transfer the alkaline solution to the alkaline side of the working fluid recovery tank. Execute Procedure Seven.

[0045] Procedure 7: Open valve 11 and valve 15, close valve 12, valve 13, and valve 16, then add 1m of water via valve 10 and the flow meter. 3 After closing valve 10, run for 30 minutes; execute procedure eight.

[0046] Procedure 8: Open valves 12, 13, and 16; close valves 11 and 15. Run for 30 minutes, allowing water droplets mixed in the working fluid to settle at the bottom as they pass through the first working fluid coalescer 5. Transfer the water to the alkaline side of the working fluid recovery tank. Repeat procedures 7 and 8 three times in total. Execute procedure 9.

[0047] Procedure Nine: Remind the user to wait for manual inspection. If there is no manual response within 20 minutes, continue to execute Procedure Seven and Procedure Eight twice. Manually sample and analyze the alkaline washing and regeneration effect of the working solution, specifically by comprehensively considering indicators such as working solution viscosity, water separation time, and anthraquinone content. If the washing and regeneration effect is met, proceed to Procedure Ten; otherwise, proceed to Procedure Eleven.

[0048] Program 10: Open valve 11 and valve 15, close valve 12, valve 13 and valve 16; execute programs 7 and 8 twice for washing; open valve 19 and add one liter of phosphoric acid through phosphoric acid metering tank 9 to prepare 40% phosphoric acid; run for 30 minutes; execute program 12.

[0049] Procedure 11: Open valve 11 and valve 15, close valve 12, valve 13, and valve 16; run procedure 5.

[0050] Procedure 12: When the pH value is detected to be ≤5, open the third valve 13, the fifth valve 15, and the seventh valve 17, and close the first valve 11 and the fifth valve 15 to send the working fluid out of the boundary area. When the pH value is detected to be 5%, close the third valve 13, the fifth valve 15, and the seventh valve 17, and open the eleventh valve 20; the first working fluid circulation pump 2 and the second working fluid circulation pump 3 stop running; and the working fluid regeneration and purification process is completed.

[0051] In summary, the following effects can be achieved by utilizing the above-described technical solution of this utility model:

[0052] 1. This alkaline washing and regeneration purification system is suitable for green and efficient all-acid hydrogen peroxide production equipment or for converting traditional acid-base hydrogen peroxide production processes into green and efficient all-acid hydrogen peroxide production processes. Since this new alkaline washing and regeneration purification system processes approximately 10 to 20 cubic meters of working liquid per day, it is well-suited for hydrogen peroxide production processes that produce less degradation products in green and efficient all-acid hydrogen peroxide production equipment.

[0053] 2. Enhanced safety: The addition of a hydrogen peroxide content analyzer and a pH analyzer to the utility model allows for direct monitoring of the hydrogen peroxide content and pH value in the working solution during alkali addition. This prevents accidents such as decomposition and explosion caused by the direct addition of alkali to the working solution with excessive hydrogen peroxide content, as is common in traditional alkali washing and regeneration systems.

[0054] 3. Compared to traditional preparation kettles, the alkali washing and regeneration purification effect is better, mainly due to the more thorough mixing of alkali solution and working solution. Firstly, it features a two-stage mixing system: a pipeline mixer and a large mixing reactor. Secondly, once alkali solution settles at the bottom of the regeneration reactor, it is immediately pumped by the working solution circulation pump to the pipeline mixer to mix with the working solution, fully utilizing the regeneration effect of the alkali solution. In contrast, in traditional preparation kettles, if some alkali solution enters the kettle, it easily settles at the bottom. The agitator is insufficient to stir up the alkali solution settled at the bottom and mix it with the working solution, failing to achieve the desired alkali washing and regeneration effect, resulting in low alkali solution utilization.

[0055] 4. Compared with traditional processes, the alkali solution and working solution are easier to separate. The working solution after washing and regenerating the alkali solution is darker in color and not much different from the color of the alkali solution used for washing. When the alkali solution is left to stand at the bottom of the preparation vessel for discharge, it is difficult to distinguish the interface between the working solution and the alkali solution with the naked eye, which easily leads to the working solution being discharged into the working solution recovery tank. However, the working solution after washing and regenerating the alkali solution has a larger density difference from the alkali solution used for washing, and it is easier to separate in the working solution coalescing tank. It can be easily discharged into the working solution recovery tank through the interface gauge control valve.

[0056] 5. This utility model can achieve a high degree of automated operation; compared with the traditional process of regenerating hydrogen peroxide from alkaline solution in the preparation tank, since there is no intermittently running agitator in the preparation tank, the degree of automation is higher and the equipment failure rate is lower.

[0057] The above are merely preferred embodiments of the present utility model and are not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model shall be included within the protection scope of the present utility model.

Claims

1. A working fluid regeneration and purification system for automated hydrogen peroxide production, characterized in that, include: The working fluid regeneration reactor (1), the first working fluid circulation pump (2), the second working fluid circulation pump (3), the working fluid filter (4), the first working fluid coalescer (5), the second working fluid coalescer (6), and the pipeline static mixer (7) are provided. The output end of the working fluid regeneration reactor (1) is connected to the input ends of the first working fluid circulation pump (2) and the second working fluid circulation pump (3), respectively. The output ends of the first working fluid circulation pump (2) and the second working fluid circulation pump (3) are connected to the input ends of the pipeline static mixer (7) and the working fluid filter (4), respectively. The output end of the working fluid filter (4) is connected to the input ends of the first working fluid coalescer (5) and the second working fluid coalescer (6), respectively. The first working fluid coalescer (5) and the second working fluid coalescer (6) are connected in parallel. The output ends of the first working fluid coalescer (5) and the second working fluid coalescer (6) are connected in parallel with the output end of the pipeline static mixer (7) and the input end of the working fluid regeneration reactor (1), respectively.

2. The hydrogen peroxide production automated operation working fluid regeneration and purification system according to claim 1, characterized in that, The output end of the working fluid regeneration reactor (1) is also connected to the alkali metering tank (8) and the phosphoric acid metering tank (9), and the alkali metering tank (8) and the phosphoric acid metering tank (9) are respectively connected to the input ends of the first working fluid circulation pump (2) and the second working fluid circulation pump (3).

3. The hydrogen peroxide production automated operation working fluid regeneration and purification system according to claim 2, characterized in that, The alkali metering tank (8) and the phosphoric acid metering tank (9) are connected to the first working fluid circulation pump (2) and the second working fluid circulation pump (3) respectively through the eighth valve (18) and the ninth valve (19).

4. The hydrogen peroxide production automated operation working fluid regeneration and purification system according to claim 1, characterized in that, The pipeline static mixer (7) is connected to the first working fluid circulation pump (2) through the first valve (11), and the pipeline static mixer (7) is connected to the working fluid filter (4) through the second valve (12).

5. The hydrogen peroxide production automated operation working fluid regeneration and purification system according to claim 1, characterized in that, The first working fluid coalescer (5) is connected to the working fluid filter (4) through the third valve (13), and the second working fluid coalescer (6) is connected to the working fluid filter (4) through the fourth valve (14).

6. The hydrogen peroxide production automated operation working fluid regeneration and purification system according to claim 1, characterized in that, The pipeline static mixer (7) is connected to the working fluid regeneration reactor (1) via the fifth valve (15).

7. The hydrogen peroxide production automated operation working fluid regeneration and purification system according to claim 1, characterized in that, The first working fluid coalescer (5) and the second working fluid coalescer (6) are connected to the working fluid regeneration reactor (1) through the sixth valve (16) and the seventh valve (17), respectively.

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