Hydrogen peroxide working solution purification system

Abstract

The utility model relates to the technical field of hydrogen peroxide chemical production, in particular to a hydrogen peroxide working solution purification system which comprises a carclazyte bed, an alkali mixing reaction device, an alkali separator, an acid mixing reaction device, an acid separator, a water washing reaction device and a water separator, the mixed liquid outlet end of the alkali mixed reaction device is connected with the liquid inlet end of the alkali separator, the organic liquid outlet end of the alkali separator is connected with the mixed liquid inlet end of the acid mixed reaction device, the mixed liquid outlet end of the acid mixed reaction device is connected with the liquid inlet end of the acid separator, and the organic liquid outlet end of the acid separator is connected with the input end of the washing reaction device; the output end of the washing reaction device is connected with the liquid inlet end of the water separator, and the organic liquid outlet end of the water separator is connected with the carclazyte bed. The activity of the carclazyte bed can be effectively prevented from being reduced, the service life of the carclazyte bed is prolonged, and the maintenance and production cost is reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of hydrogen peroxide chemical production, more particularly to a hydrogen peroxide working solution purification system. BACKGROUND

[0002] Hydrogen peroxide, scientific name hydrogen peroxide (H2O2), is mainly used in papermaking, textile, medical and other fields due to its strong oxidizing property. The preparation methods of hydrogen peroxide include electrolysis method, anthraquinone method, autoxidation method, peroxide disproportionation method and biosynthesis method, etc. In the current industrial production, the anthraquinone method is the mainstream process for producing hydrogen peroxide, which is widely used in the world due to its high efficiency, environmental protection and economic advantages. Other methods also have certain value in specific application occasions or small-scale production. At present, the reactant used in the anthraquinone method is 2-alkyl anthraquinone, and the solvent system mainly uses heavy aromatic hydrocarbon (AR) and tri-octyl phosphate (TOP) as the main components, with additional addition of other components such as tetrabutyl urea, o-methyl cyclohexyl acetate and diisobutyl methyl alcohol to form a three-solvent system. The existing process flow of hydrogen peroxide prepared by the anthraquinone method mainly includes four stages of hydrogenation reaction, oxidation reaction, extraction separation and purification, and the main reactions occur in the hydrogenation and oxidation stages. The domestic hydrogenation process mainly uses a fixed bed device. Under the action of palladium catalyst, 2-alkyl anthraquinone undergoes hydrogenation reaction under certain reaction conditions to generate intermediate 2-alkyl hydrogen anthraquinone. 2-alkyl hydrogen anthraquinone is oxidized to 2-alkyl anthraquinone and hydrogen peroxide in the subsequent oxidation process. In the hydrogenation process, 2-alkyl hydrogen anthraquinone is deeply hydrogenated to generate 2-alkyl tetrahydroanthraquinone, 2-alkyl tetrahydroanthraquinone, 2-alkyl anthrone and 2-alkyl hydroxy anthrone, etc. These by-products are collectively referred to as degradation products.

[0003] With the operation of the device, the types and contents of degradation products continue to increase, causing the consumption of 2-alkyl anthraquinone to increase, and the physicochemical properties of the hydrogen peroxide system working solution such as viscosity and surface tension also change. This not only leads to a decrease in product quality, but also poses a safety hazard to the stable operation of the system, so the working solution needs to be regenerated and purified.

[0004] However, the existing working solution regeneration and purification system widely uses a full-acid fixed bed process to regenerate the working solution using an activated clay bed. This existing technology only separates the working solution from the system at the last stage of the reaction and performs regeneration and purification treatment. On the one hand, the intermediate reactants will react with each other, which causes the waste of the intermediate reactants added. On the other hand, during the purification process, the untreated intermediate reactants will reduce the activity of the activated clay bed when they enter the activated clay bed, which leads to a decrease in the service life of the activated clay bed, frequent replacement, high maintenance and production costs. UTILITY MODEL CONTENT

[0005] The utility model discloses a hydrogen peroxide working fluid purification system which can effectively avoid the activity reduction of the white clay bed, prolong the service life of the white clay bed and reduce the maintenance and production cost.

[0006] To solve the above technical problems, the utility model adopts the technical scheme of:

[0007] The utility model provides a hydrogen peroxide working fluid purification system which comprises a white clay bed and further comprises an alkali mixing reaction device, an alkali separator, an acid mixing reaction device, an acid separator, a water washing reaction device and a water separator.

[0008] In the working process of the above scheme, the alkali reagent and the working fluid are mixed uniformly and react in the alkali mixing reaction device, the mixed liquid is input into the alkali separator through the mixing outlet end after the reaction is completed, the organic phase working fluid separated by the alkali separator is input into the acid mixing reaction device through the organic outlet end, the working fluid is mixed uniformly with the acid liquid and reacts again, the mixed liquid is input into the acid separator through the mixing outlet end after the reaction is completed, the separated organic phase working fluid is input into the water washing reaction device through the organic outlet end, and the working fluid is output to the white clay bed after water washing reaction for regeneration and purification.

[0009] Further, the utility model further comprises an alkali reagent storage tank, an acid reagent storage tank and a water storage tank, the alkali outlet end of the alkali separator is connected with the input end of the alkali reagent storage tank, the acid outlet end of the acid separator is connected with the input end of the acid reagent storage tank, and the water outlet end of the water separator is connected with the input end of the water storage tank.

[0010] Further, the alkali medicament storage tank, the acid medicament storage tank and the water storage tank are further included, the alkali outlet end of the alkali separator is connected with the input end of the alkali medicament storage tank, the acid outlet end of the acid separator is connected with the input end of the acid medicament storage tank, and the water outlet end of the water separator is connected with the input end of the water storage tank; the alkali medicament storage tank, the acid medicament storage tank and the water storage tank are respectively used for storing the collected backflow alkali medicament, acid medicament and water.

[0011] Further, the backflow blocking device is further included between the alkali medicament storage tank and the alkali separator, between the acid medicament storage tank and the acid separator, and between the water storage tank and the water separator; the backflow blocking device is used for blocking the liquid backflow of each storage tank into the separator, so as to avoid the separation failure of the separator.

[0012] Further, the output end of the acid medicament storage tank is connected with the mixed liquid inlet end of the acid mixed reaction device, and the output end of the water storage tank is connected with the input end of the water washing reaction device; after the acid medicament storage tank receives the acid medicament from the acid separator, the acid medicament storage tank can continue to input the acid medicament into the acid mixed reaction device to mix and react with the working liquid, so that the acid liquid can be recycled and used, resources are saved, and the water storage tank has the same effect.

[0013] Further, the preheating device is further included, the output end of the preheating device is connected with the mixed liquid inlet end of the alkali mixed reaction device, the reaction between the alkali medicament and the working liquid needs a certain reaction temperature, the preheating device is used for preheating the mixed liquid when the reaction is performed, so that the reaction efficiency can be effectively improved, and the target temperature range of the mixed liquid preheated by the preheating device is between 55 degrees Celsius and 85 degrees Celsius.

[0014] Further, the working liquid storage tank is further included, the output end of the alkali medicament storage tank is connected with the input end of the working liquid storage tank, and the output end of the working liquid storage tank is connected with the input end of the preheating device; the working liquid storage tank is used for storing the mixture of the working liquid and the alkali medicament, the alkali medicament recovered by the alkali medicament storage tank can continue to be input into the working liquid storage tank to mix with the working liquid, so that the alkali liquid and the working liquid can be mixed in advance, and the mixing efficiency is improved.

[0015] Further, the cooling device is further included between the alkali mixed reaction device and the alkali separator, the mixed liquid outlet end of the alkali mixed reaction device is connected with the input end of the cooling device, and the output end of the cooling device is connected with the liquid inlet end of the alkali separator; after the alkali reaction is completed, the subsequent acid reaction needs to be low, so that the mixed liquid after the alkali reaction needs to be cooled, and the temperature range of the mixed liquid at the output end of the cooling device is between 40 degrees Celsius and 60 degrees Celsius.

[0016] Further, the preheating device and the cooling device are provided with temperature and pressure control units; when the pressure is greater than 0.4 MPa and the temperature is greater than 85 DEG C, the temperature and pressure control unit controls the preheating device to stop; when the pressure is greater than 0.35 MPa and the temperature is greater than 65 DEG C, the temperature and pressure control unit controls the cooling device to stop.

[0017] Further, the underground tank is connected with the waste discharge ends of the alkali agent storage tank, the acid agent storage tank and the water storage tank; after being used for multiple times, the liquid in the alkali agent storage tank, the acid agent storage tank and the water storage tank cannot enter the reaction system again due to too many impurities, and needs to be discarded and collected to a sewage station for unified treatment through the underground tank.

[0018] Further, the acid separator and the water washing reaction device are provided with PH control units; the PH control units are used for detecting and controlling the PH value, the working liquid PH of the organic liquid outlet end of the acid separator is controlled to be between 1-5, and the working liquid PH of the organic liquid outlet end of the water separator is controlled to be between 4-6.

[0019] Compared with the prior art, the alkali agent storage tank, the acid agent storage tank, the water storage tank, the alkali mixing reaction device, the acid mixing reaction device, the water washing reaction device and the water separator are provided, the mixed liquid outlet end of the alkali mixing reaction device is connected with the liquid inlet end of the alkali separator, the organic liquid outlet end of the alkali separator is connected with the mixed liquid inlet end of the acid mixing reaction device, the mixed liquid outlet end of the acid mixing reaction device is connected with the liquid inlet end of the acid separator, the organic liquid outlet end of the acid separator is connected with the input end of the water washing reaction device, the output end of the water washing reaction device is connected with the liquid inlet end of the water separator, and the organic liquid outlet end of the water separator is connected with the white clay bed.

[0020] 1. The alkali mixing reaction device, the alkali separator, the acid mixing reaction device, the acid separator, the water washing reaction device and the water separator are provided, the mixed liquid outlet end of the alkali mixing reaction device is connected with the liquid inlet end of the alkali separator, the organic liquid outlet end of the alkali separator is connected with the mixed liquid inlet end of the acid mixing reaction device, the mixed liquid outlet end of the acid mixing reaction device is connected with the liquid inlet end of the acid separator, the organic liquid outlet end of the acid separator is connected with the input end of the water washing reaction device, the output end of the water washing reaction device is connected with the liquid inlet end of the water separator, and the organic liquid outlet end of the water separator is connected with the white clay bed.

[0021] 2. The cooling device is arranged between the alkali mixing reaction device and the alkali separator, the mixed liquid outlet end of the alkali mixing reaction device is connected with the input end of the cooling device, and the output end of the cooling device is connected with the liquid inlet end of the alkali separator; the cooling device is arranged to cool the mixture, reduce the reaction rate and improve safety. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 It is a brief flow chart of the hydrogen peroxide working liquid purification system.

[0023] Figure 2 System flow chart for Example 2;

[0024] Figure 3 System flow chart for Example 3.

[0025] In the drawings: 1, white clay bed; 2, alkali mixing reaction device; 3, alkali separator; 4, acid mixing reaction device; 5, acid separator; 6, water washing reaction device; 7, water separator; 8, alkali agent storage tank; 9, acid agent storage tank; 10, water storage tank; 11, reflux blocking device; 12, preheating device; 13, working liquid storage tank; 14, cooling device; 15, temperature and pressure control unit; 16, underground tank; 17, PH control unit. DETAILED DESCRIPTION

[0026] The utility model will be further described in connection with specific embodiments. Among them, the drawings are only for example description, show only the schematic diagram, and the physical picture, and can not be understood as the limitation of the patent; in order to better illustrate the embodiment of the utility model, some components of the drawings will be omitted, enlarged or reduced, and the size of actual product is not represented; for those skilled in the art, some well-known structure and its description in the drawings can be omitted and understood.

[0027] The same or similar reference numerals in the drawings of the embodiments of the utility model correspond to the same or similar components; in the description of the utility model, it is understood that if the orientation or position relationship indicated by the terms "upper", "lower", "left", "right" etc. is based on the orientation or position relationship shown in the drawings, only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply that the device or element must have a particular orientation, a particular orientation and operation, therefore the position relationship description in the drawings is only for example description, and can not be understood as the limitation of the patent, for the ordinary skilled in the art, the specific meaning of the above terms can be understood according to the specific situation.

[0028] Example 1

[0029] The embodiment is a first embodiment of hydrogen peroxide working liquid purification system, as shown in Figure 1As shown, the system comprises a white clay bed 1, an alkali mixing reaction device 2, an alkali separator 3, an acid mixing reaction device 4, an acid separator 5, a water washing reaction device 6, and a water separator 7. The mixing outlet of the alkali mixing reaction device 2 is connected to the liquid inlet of the alkali separator 3. The organic liquid outlet of the alkali separator 3 is connected to the mixing liquid inlet of the acid mixing reaction device 4. The mixing liquid outlet of the acid mixing reaction device 4 is connected to the liquid inlet of the acid separator 5. The organic liquid outlet of the acid separator 5 is connected to the input of the water washing reaction device 6. The output of the water washing reaction device 6 is connected to the liquid inlet of the water separator 7. The organic liquid outlet of the water separator 7 is connected to the white clay bed 1.

[0030] Specifically, as shown in Figure 2 The system further comprises an alkali agent storage tank 8, an acid agent storage tank 9, and a water storage tank 10. The alkali liquid outlet of the alkali separator 3 is connected to the input of the alkali agent storage tank 8. The acid liquid outlet of the acid separator 5 is connected to the input of the acid agent storage tank 9. The water liquid outlet of the water separator 7 is connected to the input of the water storage tank 10. The alkali agent storage tank 8, the acid agent storage tank 9, and the water storage tank 10 are used to store the collected alkali agent, acid agent, and water for subsequent reuse, thereby saving resources.

[0031] Specifically, the output of the acid agent storage tank 9 is connected to the mixing liquid inlet of the acid mixing reaction device 4. The output of the water storage tank 10 is connected to the input of the water washing reaction device 6. After receiving the acid agent from the acid separator 5, the acid agent storage tank 9 can continue to input the acid agent into the acid mixing reaction device 4 to mix with the working liquid, thereby realizing the recycling of the acid liquid and saving resources. The water storage tank 10 has the same effect.

[0032] Specifically, the system further comprises a preheating device 12. The output of the preheating device 12 is connected to the mixing liquid inlet of the alkali mixing reaction device 2. The reaction of the alkali agent and the working liquid requires a certain reaction temperature. The preheating device 12 is used to preliminarily preheat the mixed liquid during the reaction, thereby effectively improving the reaction efficiency. The target preheating temperature of the mixed liquid of the preheating device 12 ranges from 55 degrees Celsius to 85 degrees Celsius.

[0033] The working principle of the hydrogen peroxide working liquid purification system of the embodiment is as follows:

[0034] The alkali agent and the working liquid are mixed in the working liquid tank 13, preheated by the preheating device 12, and then input into the alkali mixing reaction device 2 for reaction. After the reaction is completed, the mixed liquid is input into the alkali separator 3 through the mixed liquid outlet end for separation. The organic phase working liquid separated by the alkali separator 3 is input into the acid mixing reaction device 4 through the organic liquid outlet end to mix with the acid liquid and react again. The separated alkali agent is output to the alkali agent tank 8 through the alkali liquid outlet end for recycling and storage. After the reaction in the acid mixing reaction device 4 is completed, the mixed liquid is input into the acid separator 5 through the mixed liquid outlet end for separation. The separated organic phase working liquid is input into the water washing reaction device 6 through the organic liquid outlet end. The separated acid agent is output to the acid agent tank 9 through the acid liquid outlet end for recycling and storage. After the reaction in the water washing reaction device 6 is completed, the mixed liquid is input into the water separator 7 for separation. The separated working liquid is directly input into the white clay bed 1 for regeneration and purification. The water is input into the water tank 10 for recycling and storage.

[0035] The alkali agent and the acid agent added in the whole process are separated and recycled and stored in the tank before entering the next reaction. Only the working liquid is input into the next reaction. The impurities are washed out by water before entering the white clay bed 1, and the acidity of the working liquid is reduced. Most of the intermediate reaction products of acid and alkali do not react with each other, which improves the purity of the working liquid, reduces the acidity, avoids the reduction of the activity of the white clay bed 1, prolongs the service life, and simultaneously recycles the alkali agent and the acid agent. In actual production, it is found through experiments that the working liquid directly input into the white clay bed 1 without passing through the device has a replacement cycle of 20 days / frequency. The working liquid passing through the device and then input into the white clay bed 1 for regeneration has a replacement cycle of 27 days / frequency, which effectively prolongs the service life of the white clay bed 1 and reduces the maintenance and production cost.

[0036] Example 2

[0037] The second embodiment of the hydrogen peroxide working liquid purification system is shown in Figure 2 The difference between the second embodiment and the first embodiment is that:

[0038] Specifically, the backflow blocking device 11 is installed between the alkali agent tank 8 and the alkali separator 3, between the acid agent tank 9 and the acid separator 5, and between the water tank 10 and the water separator 7. The backflow blocking device 11 is used to block the liquid in each tank from flowing back to the separator, so as to avoid the separation failure of the separator.

[0039] Specifically, the preheating device 12 and the cooling device 14 are both provided with temperature and pressure control units 15; the temperature and pressure control unit 15 controls the preheating device 12 to stop when the pressure is greater than 0.4 MPa and the temperature is greater than 85 degrees Celsius; the temperature and pressure control unit 15 controls the cooling device 14 to stop when the pressure is greater than 0.35 MPa and the temperature is greater than 65 degrees Celsius.

[0040] Specifically, the acid separator 5 and the water washing reaction device 6 are both provided with PH control units 17; the PH control units 17 are used to detect and control the PH value, the working liquid at the organic liquid outlet of the acid separator 5 is controlled to have a PH value of 1-5, and the working liquid at the organic liquid outlet of the water separator 7 is controlled to have a PH value of 4-6.

[0041] The working principle of the hydrogen peroxide working liquid purification system in the embodiment is as follows:

[0042] During the recovery and storage of the liquid in the alkali agent storage tank 8, the acid agent storage tank 9 and the water storage tank 10, as the liquid is transported, the air volume in the storage tank continuously decreases and the air pressure increases, while the air volume in the separator continuously increases, the liquid in the storage tank will backflow due to the pressure difference, and the backflow blocking device 11 can block the backflow; the temperature and pressure control unit 15 and the PH control unit 17 monitor the temperature, pressure and PH value in real time, the preheating device 12 automatically stops when the temperature and pressure exceed the safety range, and the engineer adjusts the input amount of the working liquid or water to change the PH value when the acid separator 5 and the water separator 7 do not meet the requirements.

[0043] The backflow blocking device 11 can prevent the backflow of the recovered and stored liquid into the separator during the recovery and storage process, improve the recovery efficiency, the temperature and pressure control unit 15 monitors the temperature and pressure in real time to avoid exceeding the safety range and improve safety, and the PH control unit 17 detects the PH value in real time to facilitate the engineer to understand whether the liquid in the separator meets the process requirements.

[0044] Embodiment 3

[0045] The third embodiment of the hydrogen peroxide working liquid purification system is shown in Figure 3 The difference between the embodiment and the first embodiment is that:

[0046] Specifically, the underground tank 16 is further included, and the waste discharge ends of the alkali agent storage tank 8, the acid agent storage tank 9 and the water storage tank 10 are connected with the underground tank 16; the liquid in the alkali agent storage tank 8, the acid agent storage tank 9 and the water storage tank 10 cannot enter the reaction system again after being used for multiple cycles due to too many impurities, and needs to be discarded and collected to the sewage station for unified treatment through the underground tank 16.

[0047] The working principle of the hydrogen peroxide working solution purification system of the embodiment is as follows: after the acid medicament and the alkali medicament are used repeatedly, they are input into the underground tank 16 for unified collection, and finally output to a sewage station for treatment through the underground tank 16.

[0048] The beneficial effects of the embodiment are: the cost of sewage treatment is lower, and the environment is more friendly by collecting the medicament and water which are discarded after being used repeatedly through the underground tank 16. In the specific contents of the above specific embodiments, each technical feature can be combined arbitrarily without contradiction. In order to make the description simple, all possible combinations of the above technical features are not described, however, as long as the combination of the technical features does not exist contradiction, it should be considered as the scope of the present application.

[0049] Obviously, the above embodiments of the present application are only examples for clearly illustrating the present application, and are not intended to limit the implementation modes of the present application. Based on the above description, other different forms of changes or variations can be made by those skilled in the art. Here, it is not necessary and also impossible to enumerate all the implementation modes. Any modification, equivalent replacement and improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the claims of the present application.

Claims

1. A hydrogen peroxide working solution purification system comprising a bed of white earth (1), characterized in that, The device further comprises a base mixing reaction device (2), a base separator (3), an acid mixing reaction device (4), an acid separator (5), a water washing reaction device (6) and a water separator (7), the mixing outlet end of the base mixing reaction device (2) is connected with the liquid inlet end of the base separator (3), the organic liquid outlet end of the base separator (3) is connected with the mixing liquid inlet end of the acid mixing reaction device (4), the mixing outlet end of the acid mixing reaction device (4) is connected with the liquid inlet end of the acid separator (5), the organic liquid outlet end of the acid separator (5) is connected with the input end of the water washing reaction device (6), the output end of the water washing reaction device (6) is connected with the liquid inlet end of the water separator (7), and the organic liquid outlet end of the water separator (7) is connected with the white clay bed (1).

2. The hydrogen peroxide working solution purification system of claim 1, wherein, The device further comprises a base medicament storage tank (8), an acid medicament storage tank (9) and a water storage tank (10), the base liquid outlet end of the base separator (3) is connected with the input end of the base medicament storage tank (8), the acid liquid outlet end of the acid separator (5) is connected with the input end of the acid medicament storage tank (9), and the water liquid outlet end of the water separator (7) is connected with the input end of the water storage tank (10).

3. The hydrogen peroxide working solution purification system of claim 2, wherein, The device further comprises a backflow blocking device (11), which is installed between the base medicament storage tank (8) and the base separator (3), between the acid medicament storage tank (9) and the acid separator (5), and between the water storage tank (10) and the water separator (7).

4. The hydrogen peroxide working solution purification system of claim 2, wherein, The output end of the acid medicament storage tank (9) is connected with the mixing liquid inlet end of the acid mixing reaction device (4), and the output end of the water storage tank (10) is connected with the input end of the water washing reaction device (6).

5. The hydrogen peroxide working solution purification system of claim 2, wherein, The device further comprises a preheating device (12), and the output end of the preheating device (12) is connected with the mixing liquid inlet end of the base mixing reaction device (2).

6. The hydrogen peroxide working solution purification system of claim 5, wherein, The device further comprises a working liquid storage tank (13), the output end of the base medicament storage tank (8) is connected with the input end of the working liquid storage tank (13), and the output end of the working liquid storage tank (13) is connected with the input end of the preheating device (12).

7. The hydrogen peroxide working solution purification system of claim 5, wherein, The device further comprises a cooling device (14) between the base mixing reaction device (2) and the base separator (3), the mixing outlet end of the base mixing reaction device (2) is connected with the input end of the cooling device (14), and the output end of the cooling device (14) is connected with the liquid inlet end of the base separator (3).

8. The hydrogen peroxide working solution purification system of claim 7, wherein, Temperature and pressure control units (15) are installed on the preheating device (12) and the cooling device (14).

9. The hydrogen peroxide working solution purification system of claim 2, wherein, The device further comprises an underground tank (16), and the sewage ends of the base medicament storage tank (8), the acid medicament storage tank (9) and the water storage tank (10) are connected with the underground tank (16).

10. The hydrogen peroxide working solution purification system of any one of claims 1-9, wherein, PH control units (17) are installed on the acid separator (5) and the water washing reaction device (6).

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