Safety control system for hydrogen peroxide purification

Abstract

The utility model discloses a safety control system for hydrogen peroxide purification, which comprises a resin column unit, a hydrogen peroxide unit and a regenerant unit, and the hydrogen peroxide unit and the regenerant unit are connected with an inlet end and an outlet end of the resin column unit through pipelines. On-line analyzers are arranged in outlet end pipelines, connected with the hydrogen peroxide unit and the regenerant unit, of the resin column unit, the resin column unit is connected with a sewage discharge pipeline, on-line analyzers are arranged in the sewage discharge pipeline, and three-valve groups are arranged at pipeline joints of the hydrogen peroxide unit, the regenerant unit and the resin column unit. According to the safety control system for hydrogen peroxide purification, the content of hydrogen peroxide and the content of a regenerant are monitored in real time through the online analyzer, when it is detected that the content of hydrogen peroxide or the regenerant is too high, operation is stopped, the next step is not carried out, meanwhile, three valve sets are adopted for controlling pipeline feeding, the inner leakage situation of valves can be judged easily, and the safety of hydrogen peroxide purification is improved. The mixing risk of the hydrogen peroxide and the regenerant is reduced, and accidents are prevented.

Description

Technical Field

[0001] The utility model relates to the technical field of hydrogen peroxide purification, in particular to a safety control system for hydrogen peroxide purification. Background Art

[0002] At present, the anthraquinone method is mainly used to produce hydrogen peroxide in industry. In addition to a certain amount of inorganic impurities and mechanical impurities, hydrogen peroxide produced by the anthraquinone method also contains 200-300 mg / L of organic impurities, including anthraquinone compounds and esters, alcohols, phenols, ketone compounds, etc. The domestic caprolactam production process adopts Sinopec's amine oximation process, which consumes a large amount of hydrogen peroxide in the production of caprolactam. However, if the total organic carbon content in hydrogen peroxide is too high, it will affect the quality of the finished caprolactam product at the back end, and cause catalyst poisoning, product quality degradation and excessive wastewater content. Therefore, it is necessary to purify hydrogen peroxide to reduce the organic carbon contained in hydrogen peroxide.

[0003] Related research has been conducted in the prior art, such as a new method for purifying hydrogen peroxide disclosed in Chinese patent CN111252740A, which allows hydrogen peroxide raw materials, replacement fluid A, desorption fluid, replacement fluid B, and hydrogen peroxide finished products to enter the resin column in sequence for purification and replacement. Although this method solves the problems of low resin rate and utilization efficiency, high production and processing costs in the hydrogen peroxide purification process to a certain extent, and realizes the continuous production of hydrogen peroxide purification, it does not propose corresponding safety measures for the accident risks in the hydrogen peroxide purification process. Utility Model Content

[0004] In view of this, the purpose of the utility model is to provide a safety control system for hydrogen peroxide purification, which can reduce the risk of mixing hydrogen peroxide and regeneration agent and prevent production accidents.

[0005] The utility model solves the above problems through the following technical means:

[0006] A safety control system for hydrogen peroxide purification comprises a resin column unit, a hydrogen peroxide unit and a regeneration agent unit. The hydrogen peroxide unit and the regeneration agent unit are both connected to the inlet and outlet ends of the resin column unit through pipelines. An online analyzer is arranged in the outlet pipeline connecting the resin column unit and the hydrogen peroxide unit. The resin column unit is connected to a sewage discharge pipeline, in which the online analyzer is arranged. Three valve groups are arranged at the pipeline connections between the hydrogen peroxide unit and the regeneration agent unit and the resin column unit.

[0007] Furthermore, the hydrogen peroxide unit comprises a raw hydrogen peroxide tank and a diluted hydrogen peroxide tank, and the outlet and inlet of the raw hydrogen peroxide tank and the diluted hydrogen peroxide tank are respectively connected to the two ends of the resin column unit through pipelines.

[0008] Furthermore, the regeneration agent unit includes a refined methanol tank, a recovered methanol tank, a dilute methanol tank and a crude methanol tank, the outlets and inlets of the refined methanol tank, the recovered methanol tank and the dilute methanol tank are respectively connected to the two ends of the resin column unit through pipelines, and the inlet of the crude methanol tank is connected to one end of the resin column unit through a pipeline.

[0009] Furthermore, the resin column unit is connected to a desalted water feed pipeline.

[0010] Furthermore, the resin column unit is connected to a hydrogen peroxide discharge pipeline.

[0011] Furthermore, it also includes a main controller, which is electrically connected to the online analyzer.

[0012] Furthermore, temperature control sensors are provided at the upper, middle and lower parts of the resin column unit. The resin column unit is also connected to an emergency desalted water supply pipeline and an emergency discharge pipeline. A first quick-opening valve and a second quick-opening valve are respectively provided on the emergency desalted water supply pipeline and the emergency discharge pipeline. The main controller is electrically connected to the temperature sensor, the first quick-opening valve and the second quick-opening valve, respectively.

[0013] Furthermore, the regeneration agent used in the regeneration agent unit is methanol.

[0014] Furthermore, the resin column unit includes at least two resin columns.

[0015] The utility model has at least the following beneficial effects:

[0016] 1. Use an online analyzer to monitor the content of hydrogen peroxide and regeneration agent in real time. When it is detected that the content of hydrogen peroxide or regeneration agent is too high, stop the operation and do not proceed to the next step, so as to reduce the risk of mixing hydrogen peroxide and regeneration agent and prevent accidents.

[0017] 2. Compared with the single-valve controlled feeding method of the prior art, the utility model adopts a three-valve group to control the pipeline feeding, which helps to judge the internal leakage of the valve, reduce the risk of mixing between hydrogen peroxide and regeneration agent, and prevent accidents.

[0018] 3. The regeneration agent unit adopted in the utility model includes a refined methanol tank, a recovered methanol tank, a dilute methanol tank and a crude methanol tank. Regeneration agents of different concentrations can be used to regenerate the resin column at different stages, thereby reducing the consumption of the regeneration agent and lowering the production cost.

[0019] Fourth, the main controller controls the first quick-opening valve and the second quick-opening valve in conjunction with the temperature sensor. When the temperature is too high, they are opened to discharge the hydrogen peroxide in the resin column, greatly reducing the risk of hydrogen peroxide decomposition.

[0020] 5. Compared with the existing actual resin purification production which mostly uses nitrogen to press the material, the utility model uses desalted water to press the material, which reduces the risk of decomposition of the residual hydrogen peroxide adsorbed in the resin column after nitrogen pressing. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The utility model is further described below in conjunction with the accompanying drawings and embodiments.

[0022] Figure 1 It is a schematic diagram of the safety control system for hydrogen peroxide purification.

[0023] Figure numerals: V1, resin column unit; V2, raw hydrogen peroxide tank; V3, dilute hydrogen peroxide tank; V4, refined methanol tank; V5, recovered methanol tank; V6, dilute methanol tank; V7, crude methanol tank; 1, raw hydrogen peroxide feed pipeline; 2, dilute hydrogen peroxide discharge pipeline; 3, methanol discharge pipeline; 4, emergency discharge pipeline; 5, second sewage discharge pipeline; 6, finished hydrogen peroxide discharge pipeline; 7, dilute hydrogen peroxide feed pipeline; 8, methanol feed pipeline; 9, desalted water feed pipeline; 10, emergency desalted water replenishment pipeline; 11, first sewage discharge pipeline; 12, online analyzer. DETAILED DESCRIPTION

[0024] The present invention is further described in detail below through the accompanying drawings and embodiments. Through these descriptions, the features and advantages of the present invention will become clearer and more specific. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them.

[0025] The terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the present utility model, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0026] like Figure 1 As shown, the utility model discloses a safety control system for hydrogen peroxide purification, including a resin column unit V1, a hydrogen peroxide unit and a regeneration agent unit, the hydrogen peroxide unit includes a raw hydrogen peroxide tank V2 and a dilute hydrogen peroxide tank V3, the regeneration agent unit includes a refined methanol tank V4, a recovered methanol tank V5, a dilute methanol tank V6 and a crude methanol tank V7, the regeneration agent is methanol, and the hydrogen peroxide unit and the regeneration agent unit are both connected to the inlet and outlet ends of the resin column unit V1 through pipelines.

[0027] Specifically, the outlet and inlet of the raw hydrogen peroxide tank V2 and the dilute hydrogen peroxide tank V3 are connected to the two ends of the resin column unit V1 through pipelines, respectively, the outlet and inlet of the refined methanol tank V4, the recovered methanol tank V5 and the dilute methanol tank V6 are connected to the two ends of the resin column unit V1 through pipelines, and the inlet of the crude methanol tank V7 is connected to one end of the resin column unit V1 through a pipeline. An online analyzer 12 is provided in the dilute hydrogen peroxide discharge pipeline 2 connected to the resin column unit V1 and the hydrogen peroxide unit, which is used to monitor the concentration of hydrogen peroxide flowing out of the resin column unit V1 in real time. The resin column unit V1 is also connected to a sewage discharge pipeline. The sewage discharge pipeline in this embodiment includes a first sewage discharge pipeline 11 and a second sewage discharge pipeline 5. The two have different connection parts at the resin column unit V1 and are used in conjunction with different inlet ends of the resin column unit V1, which will be further described in the subsequent process steps. An online analyzer 12 is installed in each sewage discharge pipeline. By real-time monitoring of waste liquid discharge, it can prevent high-concentration hydrogen peroxide from being discharged into the sewage pool on the one hand, and reduce the amount of water brought into the finished hydrogen peroxide on the other hand. A three-valve group is installed at the pipe connection between the hydrogen peroxide unit and the regeneration agent unit and the resin column unit V1. The three-valve group is set on the pipeline for hydrogen peroxide and regeneration agent to enter and exit the resin column, which helps to judge the internal leakage of the valve, reduce the risk of hydrogen peroxide and regeneration agent mixing, and prevent accidents.

[0028] In some embodiments, the resin column unit V1 includes at least two resin columns. In this embodiment, four resin columns are used, one for adsorption, one for regeneration, and two for standby. Alternating the use of resin columns is beneficial to improving production efficiency. Figure 1 The upper and lower ends of the resin column unit V1 can be the inlet end or the outlet end respectively. When the material is passed into one end of the resin column unit V1, it is the inlet end, and the other end is the outlet end. The inlet end and the outlet end can be switched in different production processes.

[0029] refer to Figure 1 The resin column unit V1 is connected to a desalted water feed pipeline 9, which is used to supply desalted water to the resin column for replacement. The resin column unit V1 is also connected to a finished hydrogen peroxide discharge pipeline 6, which is used to discharge the finished hydrogen peroxide after the organic carbon is removed.

[0030] In this embodiment, the safety control system for hydrogen peroxide purification also includes a main controller, which is electrically connected to the online analyzer 12. The main controller receives signals from each online analyzer 12 and stops entering the next process when abnormal concentration of hydrogen peroxide or displacer is detected, thereby improving safety.

[0031] In the present embodiment, the upper, middle and lower parts of the resin column unit V1 are provided with temperature control sensors, corresponding to the upper, middle and lower parts of each resin column. The resin column unit V1 is also connected to an emergency desalted water supply pipeline 10 and an emergency discharge pipeline 4, and a first quick-opening valve and a second quick-opening valve are respectively provided on the emergency desalted water supply pipeline 10 and the emergency discharge pipeline 4, and the main controller is electrically connected to the temperature sensor, the first quick-opening valve and the second quick-opening valve respectively. The main controller is used to control the first quick-opening valve and the second quick-opening valve in conjunction with the temperature sensor. Only when the adsorption state and the dilute hydrogen peroxide replace the raw hydrogen peroxide, the desalted water replaces the dilute hydrogen peroxide will be triggered, that is, the presence of hydrogen peroxide in the resin column will trigger, ensuring the safety of the system. When the resin column is in a state where the temperature is too high (greater than 45°C), it is opened to discharge the hydrogen peroxide in the resin column, greatly reducing the risk of hydrogen peroxide decomposition.

[0032] Combination Figure 1 The system shown in the figure further describes the process steps below, which mainly include the following steps:

[0033] Step 1, adsorption of top water: In the initial state, the resin column may contain a desalted water solution containing trace amounts of methanol. First, the raw hydrogen peroxide is used to push out the desalted water solution in the resin column to prevent the subsequent finished hydrogen peroxide from being diluted. The raw hydrogen peroxide enters the resin column from the raw hydrogen peroxide tank V2 through the raw hydrogen peroxide feed pipeline 1, and the discharge liquid is discharged from the first sewage discharge pipeline 11 of the resin column to the water service sewage pool. The first sewage discharge pipeline 11 is provided with an online analyzer 12 to monitor the discharged sewage in real time.

[0034] Step 2, organic carbon adsorption and removal: After step 1, the desalted water in the resin column has been replaced with raw hydrogen peroxide. The raw hydrogen peroxide continues to enter the resin column from the raw hydrogen peroxide tank V2 through the raw hydrogen peroxide feed pipeline 1, and the organic carbon in the raw hydrogen peroxide is adsorbed by the resin in the resin column. At this time, different from step 1, the adsorbed hydrogen peroxide is sent out through the finished hydrogen peroxide discharge pipeline 6 and finally enters the finished hydrogen peroxide tank (not shown in the figure).

[0035] Step 3, replace the raw hydrogen peroxide with dilute hydrogen peroxide: After the resin column in step 2 is saturated with organic carbon, the resin column needs to be cut out for regeneration before it can be used again. Before using the regeneration agent to regenerate the resin column, the high concentration of hydrogen peroxide in the resin column must be replaced first. Dilute hydrogen peroxide (concentration of 2%) enters the resin column from the dilute hydrogen peroxide tank V3 through the dilute hydrogen peroxide feed pipeline 7 to replace the raw hydrogen peroxide in the original resin column. The replaced raw hydrogen peroxide flows back to the raw hydrogen peroxide tank V2 through the dilute hydrogen peroxide discharge pipeline 2.

[0036] Step 4, replacing dilute hydrogen peroxide with desalted water: After step 3 is completed, the resin column contains dilute hydrogen peroxide. Desalted water enters the resin column through the desalted water feed pipeline 9, replacing the dilute hydrogen peroxide in the original resin column, and the replaced dilute hydrogen peroxide flows back to the dilute hydrogen peroxide tank V3 through the dilute hydrogen peroxide discharge pipeline 2. The online analyzer 12 provided on the dilute hydrogen peroxide discharge pipeline 2 can detect in real time to ensure that the concentration of the replaced dilute hydrogen peroxide is less than 0.5%, so as to ensure that no accidents will occur when it contacts with the regeneration agent methanol.

[0037] Step 5, resin column regeneration: The resin column is regenerated using methanol as a regeneration agent. In order to reduce the consumption of methanol and reduce production costs, three different concentrations of methanol are used for replacement regeneration. Specifically, the following steps are included:

[0038] Step 501: Recovered methanol (concentration of 50%) enters the resin column from the recovered methanol tank V5 through the methanol feed line 8, and the desalted water solution containing trace amounts of hydrogen peroxide is discharged from the second sewage discharge line 5 of the resin column to the water service sewage pool. An online analyzer 12 is provided in the second sewage discharge line 5 to prevent high-concentration methanol from being discharged into the sewage pool. Step 502: Refined methanol (concentration of 95%) enters the resin column from the refined methanol tank V4 through the methanol feed pipe to regenerate the resin, and enters the crude methanol tank V7 after being discharged from the methanol discharge pipe 3. Step 503: Dilute methanol (concentration of 10%) enters the resin column from the dilute methanol tank V6 through the methanol feed pipe to replace the refined methanol in the original resin column, and the replaced methanol is collected in the recovered methanol tank V5 through the methanol discharge line 3. The above steps complete the regeneration of the resin column. In this step, low, high, and low concentrations of methanol are used for replacement and regeneration in sequence, which can effectively reduce the methanol consumption.

[0039] Step 6, replacement of dilute methanol with desalted water: After the resin column is regenerated, dilute methanol remains in the resin column. The dilute methanol is further replaced by desalted water to return the resin column to the initial state of step 1. The desalted water is allowed to enter the resin column through the desalted water feed pipeline 9, and the dilute methanol in the original resin column is replaced and recovered, and the replaced dilute methanol is recovered to the dilute methanol tank V6 through the methanol discharge pipeline 3. Desalted water is further introduced and discharged to the water service sewage pool through the second sewage discharge pipeline 5. An online analyzer 12 is provided in the second sewage discharge pipeline 5, and the online analyzer 12 monitors the methanol concentration in real time. In step 6, the concentration of the dilute methanol replaced in the initial stage is about 10%, which can be recovered to the dilute methanol tank V6 for continued use. As the replacement process proceeds, when the methanol concentration drops to a level that is insufficient for continued recycling and use, the second sewage discharge pipeline 5 is switched to discharge the replaced solution to the water service sewage pool. Continue to replace until the methanol concentration is lower than 100ppm, and the resin column can be considered to have returned to its initial state.

[0040] In summary, the safety control system for hydrogen peroxide purification of this embodiment, combined with the above process steps, can achieve the purification of hydrogen peroxide while ensuring operational safety, while saving the consumption of various raw materials and reducing production costs.

[0041] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model rather than to limit it. Although the utility model has been described in detail with reference to the preferred embodiments, ordinary technicians in the field should understand that the technical solution of the utility model can be modified or replaced by equivalents without departing from the purpose and scope of the technical solution of the utility model, which should be included in the scope of the claims of the utility model.

Claims

1. A safety control system for hydrogen peroxide purification, characterized in that: The invention comprises a resin column unit (V1), a hydrogen peroxide unit and a regeneration agent unit. The hydrogen peroxide unit and the regeneration agent unit are connected to the inlet and outlet ends of the resin column unit (V1) through pipelines. An online analyzer (12) is arranged in the outlet pipeline connecting the resin column unit (V1) and the hydrogen peroxide unit. The resin column unit (V1) is connected to a sewage discharge pipeline, in which the online analyzer (12) is arranged. A three-valve group is arranged at the pipeline connection between the hydrogen peroxide unit and the regeneration agent unit and the resin column unit (V1).

2. The safety control system for hydrogen peroxide purification according to claim 1, characterized in that: The hydrogen peroxide unit comprises a raw hydrogen peroxide tank (V2) and a diluted hydrogen peroxide tank (V3), and the outlets and inlets of the raw hydrogen peroxide tank (V2) and the diluted hydrogen peroxide tank (V3) are respectively connected to the two ends of the resin column unit (V1) through pipelines.

3. The safety control system for hydrogen peroxide purification according to claim 2 is characterized in that: The regeneration agent unit comprises a refined methanol tank (V4), a recovered methanol tank (V5), a dilute methanol tank (V6) and a crude methanol tank (V7); the outlets and inlets of the refined methanol tank (V4), the recovered methanol tank (V5) and the dilute methanol tank (V6) are respectively connected to two ends of a resin column unit (V1) through pipelines, and the inlet of the crude methanol tank (V7) is connected to one end of the resin column unit (V1) through a pipeline.

4. The safety control system for hydrogen peroxide purification according to claim 3 is characterized in that: The resin column unit (V1) is connected to a desalted water feed pipeline (9).

5. The safety control system for hydrogen peroxide purification according to claim 4, characterized in that: The resin column unit (V1) is connected to a finished hydrogen peroxide discharge pipeline (6).

6. The safety control system for hydrogen peroxide purification according to claim 5, characterized in that: It also includes a main controller, which is electrically connected to the online analyzer (12).

7. The safety control system for hydrogen peroxide purification according to claim 6, characterized in that: The upper part, the middle part and the lower part of the resin column unit (V1) are all provided with temperature control sensors. The resin column unit (V1) is also connected to an emergency desalted water supply pipeline (10) and an emergency discharge pipeline (4). A first quick-opening valve and a second quick-opening valve are respectively provided on the emergency desalted water supply pipeline (10) and the emergency discharge pipeline (4). The main controller is electrically connected to the temperature sensor, the first quick-opening valve and the second quick-opening valve respectively.

8. The safety control system for hydrogen peroxide purification according to claim 3 is characterized in that: The regeneration agent used in the regeneration agent unit is methanol.

9. The safety control system for hydrogen peroxide purification according to any one of claims 1 to 8, characterized in that: The resin column unit (V1) includes at least two resin columns.

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