Efficient purification method for industrial frozen brine

Abstract

The invention relates to the field of frozen brine purification, in particular to an efficient purification method for industrial frozen brine. The invention relates to a high-efficiency purification method for industrial frozen brine. The method comprises the following purification steps: S1, adsorption pretreatment: taking frozen brine to be treated, and stirring the frozen brine with an adsorbent material for adsorption treatment; s2, electrodialysis purification: putting the pretreated frozen brine into an electrodialysis device for purification treatment; s3, sterilization and inactivation: carrying out ultraviolet sterilization and inactivation treatment on the frozen saline water subjected to electrodialysis purification; and S4, filtering treatment: after sterilization and inactivation are completed, filtering. According to the invention, the conductivity of the frozen brine is reduced through adsorption by the adsorbent and then electrodialysis treatment. And then ultraviolet sterilization is performed to ensure the water quality safety. In the last step, residual solid impurities are removed through a physical method, and the purity of the final product is ensured. The device realizes efficient purification of frozen brine, is suitable for industrial application, and provides reliable water quality guarantee.

Description

Technical Field

[0001] The invention relates to the field of frozen brine purification, and in particular to a high-efficiency purification method for industrial frozen brine. Background Art

[0002] At present, in industrial cooling systems, brine is used as a common refrigerant. During the circulation process, various solid impurities such as rust, sediment, corrosion products, etc. will gradually accumulate. These impurities will not only reduce the heat transfer efficiency of brine, but also cause pipe blockage and equipment damage, seriously affecting the normal operation of the refrigeration system. At present, the industry generally uses filters, centrifuges and other equipment to remove impurities in brine, but these methods often have problems such as incomplete treatment effect and high maintenance cost.

[0003] The existing methods for purifying frozen brine mainly include filter method, centrifugal separation method, sedimentation method and chemical method. Among them, the filter method intercepts solid particles in the brine by setting up multiple layers of filter screens or filter elements. This method is simple and easy to operate, but the filter screen is easy to clog and needs to be frequently cleaned or replaced, which increases maintenance costs. The centrifugal separation method uses centrifugal force to separate solid impurities with higher density from the brine. This method has a large processing capacity, but the equipment is complex, the energy consumption is high, and the removal effect of tiny particles is limited. The sedimentation method allows the solid impurities in the brine to naturally settle to the bottom by standing, and then discharges it regularly. This method takes a long time to process, occupies a large area, and is not suitable for continuous production. The chemical method adds flocculants to the brine to react with impurities to produce substances that are easy to separate. Although this method is effective, it may introduce new pollutants and cause secondary pollution to the environment and equipment.

[0004] In view of the above-mentioned prior art, the inventors found that the existing frozen brine purification method has high maintenance cost and complex process, and cannot meet the requirements of high precision and low cost. Summary of the invention

[0005] Based on the technical problems existing in the above-mentioned prior art, the present invention provides a method for efficiently purifying industrial frozen brine.

[0006] An efficient purification method for industrial frozen brine comprises the following purification steps:

[0007] S1. Adsorption pretreatment: Take the frozen brine to be treated and mix it with the adsorbent material, stir and adsorb for 15-60 minutes, and collect the pretreated frozen brine;

[0008] S2. Electrodialysis purification: The pretreated frozen brine is placed in an electrodialysis device for purification, and the voltage, current density and flow rate are adjusted until the conductivity is reduced to below the threshold;

[0009] S3, sterilization and inactivation: the frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment;

[0010] S4, filtration treatment: After the sterilization and inactivation is completed, the filtrate is filtered and collected to complete the efficient purification treatment of the industrial frozen brine.

[0011] Through the above technical scheme, the adsorption pretreatment in step S1 of the present application uses an adsorbent mixed with frozen brine, and utilizes the physical or chemical properties of the adsorbent to remove specific pollutants in the water. Different adsorbents can selectively remove different types of pollutants, thereby improving the efficiency of subsequent treatments. Next, the electrodialysis treatment in step S2 uses an electric field to drive the migration of ions in the membrane, thereby achieving the separation of salts and other ions and reducing the conductivity of the frozen brine. Step S3 effectively eliminates microorganisms in the water, especially drug-resistant bacteria and viruses, through ultraviolet sterilization to ensure water quality safety. In the last step, the filtration treatment of step S4 removes residual solid impurities by physical methods to ensure the purity of the final product. The combination of this series of steps achieves efficient purification of frozen brine, is suitable for industrial applications, and provides reliable water quality assurance.

[0012] Furthermore, the adsorbent material described in step S1 includes activated carbon powder.

[0013] Through the above technical scheme, the present application uses activated carbon powder as an adsorbent material. Activated carbon can effectively adsorb organic matter, heavy metal ions and other small molecular pollutants in water due to its rich pore structure and large specific surface area. The adsorption capacity of activated carbon not only depends on its surface properties, but is also closely related to factors such as the pH value and temperature of the solution. By adjusting the stirring time, the contact time with the frozen brine can be optimized, thereby improving the adsorption efficiency. In addition, the application of activated carbon in the treatment process is simple and economical, making it a common choice in industrial water treatment. After pretreatment, most of the pollutants in the frozen brine are removed, which provides a good foundation for the subsequent electrodialysis and ultraviolet sterilization links, and helps to improve the overall purification effect and efficiency.

[0014] Furthermore, the adsorbent material further comprises graphene oxide loaded with EDTA, and the graphene oxide loaded with EDTA is prepared by the following scheme:

[0015] Graphene is dispersed in deionized water to form a uniform suspension, ethylenediaminetetraacetic acid is added to the suspension, the pH is adjusted to 8-10, the temperature is increased, and the mixture is stirred and kept warm, centrifuged and the lower precipitate is collected, washed and dried, so as to prepare the graphene oxide loaded with EDTA.

[0016] Through the above technical solution, the present application also adds graphene oxide loaded with EDTA as an adsorbent material. Due to the two-dimensional structure and large specific surface area of ​​graphene, it can provide a higher contact area during the adsorption process, and the addition of EDTA enhances the selective removal ability of metal ions. In the preparation process of graphene, by dispersing graphene in deionized water and reacting with EDTA, EDTA can be effectively loaded to form a composite material.

[0017] Furthermore, the mass ratio of EDTA to graphene is 1:(1-5).

[0018] Through the above technical solution, the present application optimizes the composite ratio of EDTA and graphene particles, prevents excessive EDTA from causing an increase in solution viscosity, affects the dispersibility of the material and the actual use effect, and can also improve the phenomenon that insufficient EDTA cannot fully exert its complexing ability. In addition, the complexing properties of EDTA enable it to form stable complexes with a variety of metal ions, thereby improving the removal efficiency of heavy metals. This requirement provides a basis for adjusting the performance of the adsorbent in practical applications, ensuring that the ideal purification effect can be achieved in different treatment environments.

[0019] Furthermore, the graphene is graphene particles with a particle size of 100nm to 500nm.

[0020] Through the above technical scheme, the present application optimizes the particle size of graphene. Smaller particle size usually means larger specific surface area, which helps to improve adsorption capacity. However, particles that are too small may lead to poor dispersibility and strong sedimentation, thus affecting the actual application effect. Therefore, by selecting a particle size range of 100nm to 500nm, the dispersibility and fluidity of the material in water can be ensured while maintaining good adsorption. In addition, graphene particles in this particle size range also help to provide larger ion conduction channels during the electrodialysis process, thereby improving purification efficiency. This parameter provides a reference for process optimization and helps to achieve more efficient purification of frozen brine.

[0021] Furthermore, the parameters for adjusting the voltage, current density and flow rate in step S2 are: DC voltage is 10-50V, current density is 5-30mA / cm 2 , flow rate is 1-10L / h.

[0022] Through the above technical scheme, the present application adjusts the parameters of voltage, current density and flow rate to ensure efficient operation of the electrodialysis system. The principle of electrodialysis is based on electric field driven ion migration. By selecting appropriate voltage and current density, the migration speed of ions in the membrane can be effectively promoted, thereby achieving efficient salt removal and water purification. The regulation of flow rate is also crucial. Too fast flow rate may lead to insufficient ion contact time, and too slow flow rate may affect the treatment efficiency. By optimizing these parameters, the energy utilization in the electrodialysis process can be maximized and the purification effect can be improved. In addition, reasonable parameter settings help to reduce operating costs, improve the economy and practicality of the system, and adapt to industrial application needs of different scales.

[0023] Furthermore, the ultraviolet intensity of the ultraviolet sterilization treatment in step S3 is not less than 50 μW / cm 2 .

[0024] Furthermore, the filter used in the filtration in step S4 is a sieve with a pore size less than 1 μm.

[0025] In summary, this application has the following beneficial effects:

[0026] First, the adsorption pretreatment in step S1 of the present application uses an adsorbent mixed with frozen brine, and utilizes the physical or chemical properties of the adsorbent to remove specific pollutants in the water. Different adsorbents can selectively remove different types of pollutants, thereby improving the efficiency of subsequent treatments. Next, the electrodialysis treatment in step S2 uses an electric field to drive the migration of ions in the membrane, thereby achieving the separation of salts and other ions and reducing the conductivity of the frozen brine. Step S3 effectively eliminates microorganisms in the water, especially drug-resistant bacteria and viruses, through ultraviolet sterilization to ensure water safety. In the last step, the filtration treatment of step S4 removes residual solid impurities through physical methods to ensure the purity of the final product. The combination of this series of steps achieves efficient purification of frozen brine, is suitable for industrial applications, and provides reliable water quality assurance.

[0027] Second, this application uses activated carbon powder as an adsorbent material. Activated carbon can effectively adsorb organic matter, heavy metal ions and other small molecule pollutants in water due to its rich pore structure and large specific surface area. The adsorption capacity of activated carbon not only depends on its surface properties, but is also closely related to factors such as the pH value and temperature of the solution. By adjusting the stirring time, the contact time with the frozen brine can be optimized, thereby improving the adsorption efficiency. In addition, the application of activated carbon in the treatment process is simple and economical, making it a common choice in industrial water treatment. After pretreatment, most of the pollutants in the frozen brine are removed, which provides a good foundation for the subsequent electrodialysis and ultraviolet sterilization links, and helps to improve the overall purification effect and efficiency.

[0028] Third, the present application also adds graphene oxide loaded with EDTA as an adsorbent material. Due to the two-dimensional structure and large specific surface area of ​​graphene, it can provide a higher contact area during the adsorption process, and the addition of EDTA enhances the selective removal ability of metal ions. In the preparation process of graphene, by dispersing graphene in deionized water and reacting with EDTA, EDTA can be effectively loaded to form a composite material. DETAILED DESCRIPTION

[0029] The present application is further described in detail below in conjunction with embodiments.

[0030] In the examples of the present application, the raw materials and instruments used are as follows, but not limited thereto. Raw materials not otherwise specified are of analytical grade.

[0031] Preparation Example 1

[0032] Adsorbent 1

[0033] 200-500 mg of graphene with a particle size of 100 nm to 500 nm is dispersed in 500-800 g of deionized water to form a uniform suspension, ethylenediaminetetraacetic acid is added to the suspension, the mass ratio of ethylenediaminetetraacetic acid to graphene oxide is controlled to be 1:1-5, the pH is adjusted to 8-10 with a mass fraction of 1 sodium hydroxide solution, the temperature is increased to 60-80 ° C, the mixture is stirred for 3 h, centrifuged at 3000 r / min, rinsed with deionized water for 3-5 times, and then dried at 60-70 ° C for 12 h to prepare graphene loaded with EDTA.

[0034] Preparation Example 2

[0035] Adsorbent 2

[0036] Graphene was selected as the adsorbent.

[0037] Preparation Example 3

[0038] Adsorbent 3

[0039] Nano activated carbon particles are selected as adsorbent.

[0040] Example 1

[0041] An efficient purification method for industrial frozen brine comprises the following purification steps:

[0042] S1. Adsorption pretreatment: Take the frozen brine to be treated (containing suspended particles and slight microorganisms, with a total colony count of 550 CFU / mL and a turbidity of 200 NTU) and mix it with adsorbent 3 at a mass ratio of 1:100, stir and adsorb for 15 minutes, and collect the pretreated frozen brine;

[0043] S2. Electrodialysis purification: The pre-treated frozen brine is placed in an electrodialysis device for purification, with the voltage adjusted to 10V and the current density to 5mA / cm 2 and flow rate 1 L / h until the conductivity drops below the threshold;

[0044] S3. Sterilization and inactivation: The frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment, and the ultraviolet intensity is adjusted to not less than 50μW / cm 2 , irradiation time is 10-30s;

[0045] S4, filtration treatment: After the sterilization and inactivation is completed, the sieve with a pore size less than 1 μm is used for filtration and the filtrate is collected to complete the efficient purification treatment of the industrial frozen brine.

[0046] Example 2

[0047] An efficient purification method for industrial frozen brine comprises the following purification steps:

[0048] S1. Adsorption pretreatment: Take the frozen brine to be treated (containing suspended particles and slight microorganisms, with a total colony count of 550 CFU / mL and a turbidity of 200 NTU) and mix it with adsorbent 3 at a mass ratio of 1:350, stir and adsorb for 32 minutes, and collect the pretreated frozen brine;

[0049] S2. Electrodialysis purification: The pre-treated frozen brine is placed in an electrodialysis device for purification, with the voltage adjusted to 35V and the current density to 18mA / cm 2 and flow rate 6 L / h until the conductivity drops below the threshold;

[0050] S3. Sterilization and inactivation: The frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment, and the ultraviolet intensity is adjusted to not less than 50μW / cm 2 , irradiation time is 20s;

[0051] S4, filtration treatment: After the sterilization and inactivation is completed, the sieve with a pore size less than 1 μm is used for filtration and the filtrate is collected to complete the efficient purification treatment of the industrial frozen brine.

[0052] Example 3

[0053] An efficient purification method for industrial frozen brine comprises the following purification steps:

[0054] S1. Adsorption pretreatment: Take the frozen brine to be treated (containing suspended particles and slight microorganisms, with a total colony count of 550 CFU / mL and a turbidity of 200 NTU) and mix it with adsorbent 3 at a mass ratio of 1:500, stir and adsorb for 60 minutes, and collect the pretreated frozen brine;

[0055] S2. Electrodialysis purification: The pre-treated frozen brine is placed in an electrodialysis device for purification, with the voltage adjusted to 50V and the current density to 30mA / cm 2 and flow rate 10 L / h until the conductivity drops below the threshold;

[0056] S3. Sterilization and inactivation: The frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment, and the ultraviolet intensity is adjusted to not less than 50μW / cm 2 , irradiation time is 30s;

[0057] S4, filtration treatment: After the sterilization and inactivation is completed, the sieve with a pore size less than 1 μm is used for filtration and the filtrate is collected to complete the efficient purification treatment of the industrial frozen brine.

[0058] Example 4

[0059] An efficient purification method for industrial frozen brine comprises the following purification steps:

[0060] S1. Adsorption pretreatment: Take the frozen brine to be treated (containing suspended particles and slight microorganisms, with a total colony count of 550 CFU / mL and a turbidity of 200 NTU) and mix it with adsorbent 2 at a mass ratio of 1:350, stir and adsorb for 32 minutes, and collect the pretreated frozen brine;

[0061] S2, electrodialysis purification: the pre-treated frozen brine is placed in an electrodialysis device for purification, the voltage is adjusted to 35V, the current density is 18mA / cm2 and the flow rate is 6L / h, and the conductivity is reduced to below the threshold;

[0062] S3. Sterilization and inactivation: The frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment, and the ultraviolet intensity is adjusted to not less than 50μW / cm 2 , irradiation time is 20s;

[0063] S4, filtration treatment: After the sterilization and inactivation is completed, the sieve with a pore size less than 1 μm is used for filtration and the filtrate is collected to complete the efficient purification treatment of the industrial frozen brine.

[0064] Example 5

[0065] An efficient purification method for industrial frozen brine comprises the following purification steps:

[0066] S1. Adsorption pretreatment: Take the frozen brine to be treated (containing suspended particles and slight microorganisms, with a total colony count of 550 CFU / mL and a turbidity of 200 NTU) and mix it with adsorbent 1 at a mass ratio of 1:350, stir and adsorb for 32 minutes, and collect the pretreated frozen brine;

[0067] S2, electrodialysis purification: the pre-treated frozen brine is placed in an electrodialysis device for purification, the voltage is adjusted to 35V, the current density is 18mA / cm2 and the flow rate is 6L / h, and the conductivity is reduced to below the threshold;

[0068] S3. Sterilization and inactivation: The frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment, and the ultraviolet intensity is adjusted to not less than 50μW / cm 2 , irradiation time is 20s;

[0069] S4, filtration treatment: After the sterilization and inactivation is completed, the sieve with a pore size less than 1 μm is used for filtration and the filtrate is collected to complete the efficient purification treatment of the industrial frozen brine.

[0070] Performance Testing

[0071] The performance of the purified frozen brine of Examples 1-5 was tested, specifically the total bacteria count and turbidity thereof, and the test method was as follows:

[0072] Total bacterial count: Dilute the water sample appropriately, spread it on a plate culture medium, and culture it at 37°C under aerobic conditions for 48 hours. Count the number of colonies on the plate and multiply it by the dilution factor to calculate the total number of bacteria in the water sample.

[0073] Turbidity: tested with WZS-190S turbidity meter. The results are shown in Table 1 below:

[0074] Table 1 Performance test table

[0075]

[0076] From the above examples 1-3, combined with the test results in Table 1, it can be found that:

[0077] The adsorption pretreatment in step S1 of the present application uses an adsorbent mixed with frozen brine, and utilizes the physical or chemical properties of the adsorbent to remove specific pollutants in the water. Different adsorbents can selectively remove different types of pollutants, thereby improving the efficiency of subsequent treatments. Next, the electrodialysis treatment in step S2 uses an electric field to drive the migration of ions in the membrane, thereby achieving the separation of salts and other ions and reducing the conductivity of the frozen brine. Step S3 effectively eliminates microorganisms in the water, especially drug-resistant bacteria and viruses, through ultraviolet sterilization to ensure water quality safety. In the last step, the filtration treatment of step S4 removes residual solid impurities through physical methods to ensure the purity of the final product. The combination of this series of steps achieves efficient purification of frozen brine, is suitable for industrial applications, and provides reliable water quality assurance.

[0078] Secondly, by comparing Examples 1-3, Example 4 and Example 5, it can be found that the present application adds graphene oxide loaded with EDTA as an adsorbent material. Due to the two-dimensional structure and large specific surface area of ​​graphene, it can provide a higher contact area during the adsorption process, and the addition of EDTA enhances the selective removal ability of metal ions.

[0079] The present invention has been described in detail above in conjunction with specific implementations and exemplary examples, but these descriptions cannot be understood as limiting the present invention. Those skilled in the art understand that, without departing from the spirit and scope of the present invention, a variety of equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its implementation methods, all of which fall within the scope of the present invention. The scope of protection of the present invention shall be subject to the attached claims.

[0080] All publications, patent applications, patents and other references mentioned in this specification are incorporated herein by reference. Unless otherwise defined, all technical and scientific terms used in this specification have the meanings conventionally understood by those skilled in the art. In the event of a conflict, the definition in this specification shall prevail.

[0081] When this specification uses the prefix "well-known to those skilled in the art", "prior art" or similar terms to introduce materials, substances, methods, steps, devices or components, etc., the objects introduced by the prefix cover those commonly used in the art when this application is filed, but also include those that are not commonly used at present but will become recognized in the art as being suitable for similar purposes.

[0082] In the context of the present specification, any matters or items not mentioned are directly applicable to those known in the art without any changes except those explicitly stated.

Claims

1. A highly efficient purification method for industrial frozen brine, characterized in that: The purification steps include: S1. Adsorption pretreatment: Take the frozen brine to be treated and mix it with the adsorbent material, stir and adsorb for 15-60 minutes, and collect the pretreated frozen brine; S2. Electrodialysis purification: The pretreated frozen brine is placed in an electrodialysis device for purification, and the voltage, current density and flow rate are adjusted until the conductivity is reduced to below the threshold; S3, sterilization and inactivation: the frozen brine after electrodialysis purification is subjected to ultraviolet sterilization and inactivation treatment; S4, filtration treatment: After the sterilization and inactivation is completed, the filtrate is filtered and collected to complete the efficient purification treatment of the industrial frozen brine.

2. A highly efficient purification method for industrial frozen brine according to claim 1, characterized in that: The adsorbent material described in step S1 includes activated carbon powder.

3. A highly efficient purification method for industrial frozen brine according to claim 2, characterized in that: The adsorbent material also includes graphene oxide loaded with EDTA, and the graphene oxide loaded with EDTA is prepared by the following scheme: Graphene is dispersed in deionized water to form a uniform suspension, ethylenediaminetetraacetic acid is added to the suspension, the pH is adjusted to 8-10, the temperature is increased, and the mixture is stirred and kept warm, centrifuged and the lower precipitate is collected, washed and dried, so as to prepare the graphene oxide loaded with EDTA.

4. A highly efficient purification method for industrial frozen brine according to claim 3, characterized in that: The mass ratio of EDTA to graphene is 1:(1-5).

5. The method for efficiently purifying industrial frozen brine according to claim 3, characterized in that: The graphene is graphene particles with a particle size of 100nm to 500nm.

6. The method for efficiently purifying industrial frozen brine according to claim 1, characterized in that: The parameters for adjusting the voltage, current density and flow rate in step S2 are: DC voltage of 10-50V, current density of 5-30mA / cm 2 , flow rate is 1-10L / h.

7. The method for efficiently purifying industrial frozen brine according to claim 1, characterized in that: The ultraviolet intensity of the ultraviolet sterilization treatment described in step S3 is not less than 50 μW / cm 2 .

8. The method for efficiently purifying industrial frozen brine according to claim 1, characterized in that: The filter used in the filtration in step S4 is a sieve with a pore size less than 1 μm.

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