Purifying and washing process for hydrogen peroxide working solution

Abstract

The invention relates to the technical field of chemical production, in particular to a hydrogen peroxide working solution purifying and washing process. Comprising the following steps: S1, constructing a hydrogen peroxide working solution purifying and washing system; s2, injecting the working solution into a stock solution kettle in a hydrogen peroxide working solution purifying and washing system for reaction, and then carrying out solid-liquid separation; s3, performing dissolution treatment on a product obtained through solid-liquid separation; s4, after the dissolving treatment is completed, washing with water, performing secondary separation when precipitates appear in the liquid, and temporarily storing the obtained separation liquid; s5, purifying the carclazyte bed in the washing system by using the hydrogen peroxide working solution to separate residual substances, recombining effective component substances, and finally regenerating and temporarily storing a finished product; according to the invention, the production speed of octahydro-anthraquinone in the working solution is reduced, the conversion or extraction process of octahydro-anthraquinone is improved, the purpose of reducing by-product components in the working solution to be controllable is realized, the reaction activity of the working solution is improved, the production consumption is reduced, and long-period safe and stable operation of the device is realized.

Description

Technical Field

[0001] The invention relates to the technical field of chemical production, in particular to a purification and washing process of a hydrogen peroxide working solution. Background Art

[0002] In the anthraquinone method of hydrogen peroxide production, the carrier anthraquinone in the working liquid undergoes a certain degree of side reaction while undergoing the main reaction (hydrogenation reaction, oxidation reaction), forming anthraquinone by-products (i.e. degradation products). There is currently no effective regeneration treatment method for hydrogenated by-products (octahydroanthraquinone, decahydroanthraquinone, etc.) at home and abroad. As the operating cycle of the device increases, impurities in the working liquid gradually accumulate, causing the state of the working liquid to gradually deteriorate. This results in a decrease in effective anthraquinone in the working liquid and a reduction in the production capacity of the device. The density and viscosity of the working liquid increase, and the efficiency of the extraction tower decreases, resulting in a high content of water in the working liquid and residual hydrogen peroxide, which poses a greater safety risk.

[0003] During the operation of the working fluid, octahydroanthraquinone circulates ineffectively and accumulates in the system in the form of octahydroanthraquinone, causing the working fluid to deteriorate: the viscosity is high, anthraquinone is easy to precipitate, the surface tension becomes smaller, and the density increases, which increases the burden on the filtration system and affects the oil-water separation effect of the extraction tower, resulting in high water content in the working fluid and residual hydrogen peroxide content, posing a greater safety risk, and making it difficult to maintain continuous production of the device.

[0004] Based on this, the present invention provides a hydrogen peroxide working solution purification and washing process to solve the above-mentioned technical problems. Summary of the invention

[0005] The object of the present invention is to provide a hydrogen peroxide working fluid purification and washing process, which adopts different methods to purify the working fluid, so that the effective anthraquinone in the working fluid is increased, thereby improving the production capacity of the device; reducing the density and viscosity of the working fluid, reducing the water and hydrogen peroxide content in the working fluid, and reducing the safety risks during the operation of the production device.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention provides a hydrogen peroxide working solution purification and washing process, comprising the following steps:

[0008] S1. Construct a hydrogen peroxide working fluid purification and washing system;

[0009] S2, injecting the working liquid into the stock liquid kettle in the hydrogen peroxide working liquid purification and washing system for reaction, and then separating the solid and liquid;

[0010] S3, dissolving the product obtained through solid-liquid separation;

[0011] S4, after the dissolution treatment is completed, washing with water, when precipitates appear in the liquid, secondary separation, and temporary storage of the obtained separated liquid;

[0012] S5. Use hydrogen peroxide working solution to purify the clay bed in the washing system to separate the residual substances, and recombine the effective component substances, and finally regenerate them and temporarily store the finished products.

[0013] The present invention is further configured as follows: in step S1, the hydrogen peroxide working solution purification and washing system comprises a stock solution kettle, a configuration kettle B, a bleaching clay bed and an ice source storage tank, wherein:

[0014] The output end of the stock liquid kettle is connected to a filter press separator, and the output end of the filter press separator is connected to a configuration kettle A;

[0015] The output end of the configuration kettle B is connected to the input end of the configuration kettle A, the output end of the configuration kettle B is connected to a mixing kettle, the output end of the mixing kettle is connected to a receiving tank, and the output end of the receiving tank is connected to a catalyst configuration box;

[0016] The input end of the clay bed is connected to the catalyst configuration box, the output end of the clay bed is connected to the catalyst regeneration bed, and a circulation pump is installed on the clay bed;

[0017] The output end of the stock liquid kettle is connected to an exchanger, the output end of the exchanger is connected to an ice source storage tank, the output end of the exchanger is connected to a solvent kettle, and the output end of the solvent kettle is connected to a delivery pump;

[0018] The ice source storage tank is communicated with the stock liquid kettle, the ice source storage tank is connected to an ice machine, and the ice machine is connected to a cooler.

[0019] The present invention is further configured as follows: the input end of the configuration kettle B is connected to a balance calculator, and the configuration kettle B is communicated with the solvent kettle.

[0020] The present invention is further configured as follows: the input end of the mixing kettle is connected to a weighing scale, and the input end of the weighing scale is connected to a liquid storage tank.

[0021] The present invention is further configured such that: the output end of the catalyst configuration box is connected to a receiver.

[0022] The present invention is further configured as follows: in step S2, the reaction process is to heat the working liquid to 73-77° C. and leave it to stand for 4 hours.

[0023] The present invention is further configured as follows: in step S3, the dissolution process is as follows:

[0024] After the temperature is raised to 60°C, 3-7% of the mass of the product extract is added thereto, and the temperature is raised to 75°C, and the mixture is allowed to stand for 30 minutes;

[0025] Then, a reducing agent was added thereto, and the mixture was stirred for 40 minutes.

[0026] The present invention is further configured as follows: the extract is a mixture of phosphoric acid and pure water.

[0027] The present invention is further configured as follows: in step S4, the separation liquid is temporarily stored at a temperature of 39-41°C.

[0028] The present invention is further configured as follows: in step S4, the water washing is completed by adding pure water, stirring, and standing still, wherein the amount of pure water added is 3% of the amount of solvent, the rotation speed is 17r / min, the stirring time is 2h, and the standing time is 30min.

[0029] The present invention is further configured as follows: in step S5, the separation time is 2 hours.

[0030] The present invention is further configured as follows: in the step S5, the temperature of the recombination is 40° C., and the stirring is performed for 1 hour.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] The present invention reduces the generation rate of octahydroanthraquinone in the working solution, improves the conversion or extraction process of octahydroanthraquinone, and achieves the purpose of reducing the by-product components in the working solution to a controllable level, thereby improving the reaction activity of the working solution, reducing production consumption, and realizing long-term safe and stable operation of the device. The hydrogen peroxide working solution purification and washing process provided by the present invention has broad application prospects and is worthy of promotion. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a system diagram of the hydrogen peroxide working solution purification and washing system in Example 1.

[0034] Description of Figure Numbers:

[0035] 1. Raw liquid kettle; 2. Filter press separator; 3. Configuration kettle A; 4. Configuration kettle B; 5. Mixing kettle; 6. Receiving tank; 7. Catalyst configuration box; 8. Receiver; 9. White clay bed; 10. Circulation pump; 11. Catalyst regeneration bed; 12. Balance calculator; 13. Weighing scale; 14. Liquid storage tank; 15. Exchanger; 16. Solvent kettle; 17. Delivery pump; 18. Cooler; 19. Ice machine; 20. Ice source storage tank. DETAILED DESCRIPTION

[0036] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] Example 1

[0038] like Figure 1 As shown, in order to realize the purification and washing of the hydrogen peroxide working solution of the present invention, this embodiment provides a hydrogen peroxide working solution purification and washing system, which includes a stock liquid kettle 1, a configuration kettle B4, a white clay bed 9 and an ice source storage tank 20, wherein: the output end of the stock liquid kettle 1 is connected to a filter press separator 2, and the output end of the filter press separator 2 is connected to a configuration kettle A3; the output end of the configuration kettle B4 is connected to the input end of the configuration kettle A3, the output end of the configuration kettle B4 is connected to a mixing kettle 5, the output end of the mixing kettle 5 is connected to a receiving tank 6, and the output end of the receiving tank 6 is connected to Catalyst configuration box 7; the input end of the kaolin bed 9 is connected to the catalyst configuration box 7, the output end of the kaolin bed 9 is connected to the catalyst regeneration bed 11, and a circulation pump 10 is installed on the kaolin bed 9; the output end of the stock liquid kettle 1 is connected to the exchanger 15, the output end of the exchanger 15 is connected to the ice source storage tank 20, the output end of the exchanger 15 is connected to the solvent kettle 16, and the output end of the solvent kettle 16 is connected to the delivery pump 17; the ice source storage tank 20 is connected to the stock liquid kettle 1, the ice source storage tank 20 is connected to the ice machine 19, and the ice machine 19 is connected to the cooler 18.

[0039] In this embodiment, it should be noted that the working liquid to be treated will be sent to the stock liquid kettle 1. As a feasible implementation method, a centrifugal pump can be used to pump the working liquid into the stock liquid kettle 1, wherein the working liquid components mainly include aromatic hydrocarbons, TBU / TOP, anthraquinone, hydroanthraquinone, epoxides, anthrone and degradation products, etc. The filter press separator 2 provided can perform solid-liquid separation on the materials received from the stock liquid kettle 1, and discharge the impurities, which are mainly anthrone and degradation products, etc., and then send them to the configuration kettle A3. After being treated in the configuration kettle A3, they will be sent to the mixing kettle 5 for water washing. In addition, the exchanger 15 provided is used for cold and heat exchange, and the distillate of the solvent kettle 16 is treated and then sent to the configuration kettle B4, and then enters the configuration kettle A3.

[0040] Furthermore, the input end of the configuration kettle B4 is connected to a balance calculator 12, and the configuration kettle B4 is connected to the solvent kettle 16. The input end of the mixing kettle 5 is connected to a weighing scale 13, and the input end of the weighing scale 13 is connected to a liquid storage tank 14. The output end of the catalyst configuration box 7 is connected to a receiver 8.

[0041] In this embodiment, it should be noted that a quantitative amount of balancing agent can be sent into the configuration kettle B4 through the balance calculator 12, and after the working liquid is processed, it is sent into the configuration kettle A3; pure water can be stored in the liquid storage tank 14, and after being weighed by the measuring scale 13, it is sent into the mixing kettle 5 and washed with water in the mixing kettle 5.

[0042] Example 2

[0043] This embodiment provides a hydrogen peroxide working solution purification and washing process, comprising the following steps:

[0044] S1. Construct a hydrogen peroxide working fluid purification and washing system.

[0045] In this embodiment, it should be noted that the system is the hydrogen peroxide working fluid purification and washing system in Example 1.

[0046] S2, injecting the working liquid into the stock liquid kettle 1 in the hydrogen peroxide working liquid purification and washing system for reaction, and then separating the solid and the liquid.

[0047] The reaction process is to heat the working solution to 73°C and leave it to stand for 4 hours.

[0048] S3, dissolving the product obtained after solid-liquid separation.

[0049] The dissolution process is as follows:

[0050] After the temperature is raised to 60°C, 3% of the mass of the product extract is added thereto, and the temperature is raised to 75°C, and the mixture is allowed to stand for 30 minutes;

[0051] Then, a reducing agent was added thereto, and the mixture was stirred for 40 minutes.

[0052] The present invention is further configured as follows: the extract is a mixture of phosphoric acid and pure water.

[0053] S4. After the dissolution treatment is completed, wash with water, and when a precipitate appears in the liquid, separate it for the second time, and temporarily store the separated liquid.

[0054] The temporary storage temperature of the separation liquid is 39°C.

[0055] The water washing is completed by adding pure water, stirring, and standing still, wherein the amount of pure water added is 3% of the amount of solvent, the rotation speed is 17r / min, the stirring time is 2h, and the standing time is 30min.

[0056] In this embodiment, it should be noted that the specific substances of the precipitates include octahydroanthraquinone, tetrahydroanthraquinone, polyhydrogen compounds, degradation products, etc.

[0057] S5. Use hydrogen peroxide working solution to purify the clay bed 9 in the washing system to separate the residual substances, and recombine the effective component substances, and finally regenerate them and temporarily store the finished products.

[0058] The separation time is 2h.

[0059] The recombinant temperature was 40°C and the mixture was stirred for 1 h.

[0060] In this embodiment, it should be noted that the residual substances are separated by entering the acidic clay, wherein the acidic clay is modified activated alumina, which has spherical, honeycomb, powdery and the like shapes; and the working fluid can reach a qualified state after regeneration.

[0061] Example 3

[0062] This embodiment provides a hydrogen peroxide working solution purification and washing process, comprising the following steps:

[0063] S1. Construct a hydrogen peroxide working fluid purification and washing system.

[0064] In this embodiment, it should be noted that the system is the hydrogen peroxide working fluid purification and washing system in Example 1.

[0065] S2, injecting the working liquid into the stock liquid kettle 1 in the hydrogen peroxide working liquid purification and washing system for reaction, and then separating the solid and the liquid.

[0066] The reaction process is to heat the working solution to 75°C and leave it to stand for 4 hours.

[0067] S3, dissolving the product obtained after solid-liquid separation.

[0068] The dissolution process is as follows:

[0069] After the temperature is raised to 60°C, 5% of the mass of the product extract is added thereto, and the temperature is raised to 75°C, and the mixture is allowed to stand for 30 minutes;

[0070] Then, a reducing agent was added thereto, and the mixture was stirred for 40 minutes.

[0071] The present invention is further configured as follows: the extract is a mixture of phosphoric acid and pure water.

[0072] S4. After the dissolution treatment is completed, wash with water, and when a precipitate appears in the liquid, separate it for the second time, and temporarily store the separated liquid.

[0073] The temporary storage temperature of the separation liquid is 40°C.

[0074] The water washing is completed by adding pure water, stirring, and standing still, wherein the amount of pure water added is 3% of the amount of solvent, the rotation speed is 17r / min, the stirring time is 2h, and the standing time is 30min.

[0075] In this embodiment, it should be noted that the specific substances of the precipitates include octahydroanthraquinone, tetrahydroanthraquinone, polyhydrogen compounds, degradation products, etc.

[0076] S5. Use hydrogen peroxide working solution to purify the clay bed 9 in the washing system to separate the residual substances, and recombine the effective component substances, and finally regenerate them and temporarily store the finished products.

[0077] The separation time is 2h.

[0078] The recombinant temperature was 40°C and the mixture was stirred for 1 h.

[0079] In this embodiment, it should be noted that the residual substances are separated by entering the acidic clay, wherein the acidic clay is modified activated alumina, which has spherical, honeycomb, powdery and the like shapes; and the working fluid can reach a qualified state after regeneration.

[0080] Example 4

[0081] This embodiment provides a hydrogen peroxide working solution purification and washing process, comprising the following steps:

[0082] S1. Construct a hydrogen peroxide working fluid purification and washing system.

[0083] In this embodiment, it should be noted that the system is the hydrogen peroxide working fluid purification and washing system in Example 1.

[0084] S2, injecting the working liquid into the stock liquid kettle 1 in the hydrogen peroxide working liquid purification and washing system for reaction, and then separating the solid and the liquid.

[0085] The reaction process is to heat the working solution to 77°C and leave it to stand for 4 hours.

[0086] S3, dissolving the product obtained after solid-liquid separation.

[0087] The dissolution process is as follows:

[0088] After the temperature is raised to 60°C, 7% of the mass of the product extract is added thereto, and the temperature is raised to 75°C, and the mixture is allowed to stand for 30 minutes;

[0089] Then, a reducing agent was added thereto, and the mixture was stirred for 40 minutes.

[0090] The present invention is further configured as follows: the extract is a mixture of phosphoric acid and pure water.

[0091] S4. After the dissolution treatment is completed, wash with water, and when a precipitate appears in the liquid, separate it for the second time, and temporarily store the separated liquid.

[0092] The temporary storage temperature of the separation liquid is 41°C.

[0093] The water washing is completed by adding pure water, stirring, and standing still, wherein the amount of pure water added is 3% of the amount of solvent, the rotation speed is 17r / min, the stirring time is 2h, and the standing time is 30min.

[0094] In this embodiment, it should be noted that the specific substances of the precipitates include octahydroanthraquinone, tetrahydroanthraquinone, polyhydrogen compounds, degradation products, etc.

[0095] S5. Use hydrogen peroxide working solution to purify the clay bed 9 in the washing system to separate the residual substances, and recombine the effective component substances, and finally regenerate them and temporarily store the finished products.

[0096] The separation time is 2h.

[0097] The recombinant temperature was 40°C and the mixture was stirred for 1 h.

[0098] In this embodiment, it should be noted that the residual substances are separated by entering the acidic clay, wherein the acidic clay is modified activated alumina, which has spherical, honeycomb, powdery and the like shapes; and the working fluid can reach a qualified state after regeneration.

[0099] Performance testing:

[0100] Based on the system of Example 1, Examples 2 to 4 were used to treat the working fluid of this process, and chemical tests were performed respectively, wherein Example 2 used the working fluid of September 13, Example 3 used the working fluid of September 30, and Example 4 used the working fluid of October 9.

[0101] Table 1: Chemical testing data record table

[0102]

[0103]

[0104] As shown in Table 1, the total content of octahydroanthraquinone is effectively reduced and the effective anthraquinone of the working solution is increased by comparing the components of the working solution before and after. At the same time, the anthraquinone degradation products and 22min unknown substances in the working solution are also effectively removed, and the production efficiency is improved and the production cost is reduced. In addition, when the working solution is disposed, it can be disposed in batches, and the hydrogen peroxide production device does not stop and does not affect normal operation, thereby stabilizing the output of hydrogen peroxide.

[0105] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0106] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A hydrogen peroxide working solution purification and washing process, characterized in that: The following steps are involved: S1. Construct a hydrogen peroxide working fluid purification and washing system; S2, injecting the working liquid into the stock liquid kettle (1) in the hydrogen peroxide working liquid purification and washing system for reaction, and then separating the solid and liquid; S3, dissolving the product obtained through solid-liquid separation; S4, after the dissolution treatment is completed, washing with water, when precipitates appear in the liquid, secondary separation, and temporary storage of the obtained separated liquid; S5. Using hydrogen peroxide working solution to purify the clay bed (9) in the washing system to separate the residual substances, and to recombine the effective component substances, and finally to regenerate and temporarily store the finished product.

2. The hydrogen peroxide working solution purification and washing process according to claim 1, characterized in that: In step S1, the hydrogen peroxide working solution purification and washing system comprises a stock solution kettle (1), a configuration kettle B (4), a white clay bed (9) and an ice source storage tank (20), wherein: The output end of the stock liquid kettle (1) is connected to a filter press separator (2), and the output end of the filter press separator (2) is connected to a configuration kettle A (3); The output end of the configuration kettle B (4) is connected to the input end of the configuration kettle A (3), the output end of the configuration kettle B (4) is connected to a mixing kettle (5), the output end of the mixing kettle (5) is connected to a receiving tank (6), and the output end of the receiving tank (6) is connected to a catalyst configuration box (7); The input end of the clay bed (9) is connected to the catalyst configuration box (7), the output end of the clay bed (9) is connected to the catalyst regeneration bed (11), and a circulation pump (10) is installed on the clay bed (9); The output end of the stock liquid kettle (1) is connected to an exchanger (15), the output end of the exchanger (15) is connected to an ice source storage tank (20), the output end of the exchanger (15) is connected to a solvent kettle (16), and the output end of the solvent kettle (16) is connected to a delivery pump (17); The ice source storage tank (20) is in communication with the raw liquid kettle (1), the ice source storage tank (20) is connected to an ice machine (19), and the ice machine (19) is connected to a cooler (18).

3. The hydrogen peroxide working solution purification and washing process according to claim 2, characterized in that: The input end of the configuration kettle B (4) is connected to a balance calculator (12), and the configuration kettle B (4) is in communication with a solvent kettle (16).

4. The hydrogen peroxide working solution purification and washing process according to claim 2, characterized in that: The input end of the mixing kettle (5) is connected to a weighing scale (13), and the input end of the weighing scale (13) is connected to a liquid storage tank (14).

5. The hydrogen peroxide working solution purification and washing process according to claim 2, characterized in that: The output end of the catalyst configuration box (7) is connected to a receiver (8).

6. The hydrogen peroxide working solution purification and washing process according to claim 1, characterized in that: In step S2, the reaction process is to heat the working solution to 73-77° C. and leave it to stand for 4 hours.

7. The hydrogen peroxide working solution purification and washing process according to claim 1, characterized in that: In step S3, the dissolution process is as follows: After the temperature is raised to 60°C, 3-7% of the mass of the product extract is added thereto, and the temperature is raised to 75°C, and the mixture is allowed to stand for 30 minutes; Then, a reducing agent was added thereto, and the mixture was stirred for 40 minutes.

8. The hydrogen peroxide working solution purification and washing process according to claim 1, characterized in that: In step S4, the separation liquid is temporarily stored at a temperature of 39-41°C.

9. The hydrogen peroxide working solution purification and washing process according to claim 1, characterized in that: In step S5, the separation time is 2 hours.

10. The hydrogen peroxide working solution purification and washing process according to claim 1, characterized in that: In the step S5, the recombining temperature is 40° C. and the stirring is performed for 1 hour.

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