Sulfonamide antibiotic efficient adsorbent as well as preparation method and application thereof

By using tetrabenzyl phosphate as a monomer, porous adsorbents were prepared through Friedel-Crafts alkylation reaction, the problem of the unsatisfactory adsorption efficiency of existing porous materials for sulfonamide antibiotics was solved, and efficient and rapid adsorption effect was achieved, and good regeneration and recycling performance was achieved.

CN119680514APending Publication Date: 2025-03-25JINGCHU UNIV OF TECH
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Patent Information

Application Number
CN202411595983.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-11
Publication Date
2025-03-25

AI Technical Summary

Technical Problem

The adsorption efficiency of existing porous materials to sulfonamide antibiotics is not ideal, resulting in a small adsorption amount and slow adsorption rate, and a complex preparation process and high cost.

Method used

Using tetrabenzyl phosphate as a monomer, a porous adsorbent was prepared by Friedel-Crafts alkylation reaction, increasing the specific surface area and porosity, and improving the adsorption rate.

Benefits of technology

The prepared adsorbent has a high specific surface area and a multi-stage pore structure, which can efficiently adsorb a variety of sulfonamide antibiotics, with a fast adsorption rate and a high adsorption amount after multiple regeneration treatments.

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Abstract

The invention discloses a preparation method of a sulfonamide antibiotic efficient adsorbent, which comprises the following steps: adding tetrabenzyl phosphate, a cross-linking agent, an auxiliary agent and a catalyst into a solvent according to a certain proportion, and carrying out Friedel-Crafts alkylation reaction at a certain temperature to obtain a product; and purifying the product to obtain the porous adsorbent. The prepared efficient adsorbent for the sulfonamide antibiotics has a relatively high specific surface area and a hierarchical pore structure, contains rich oxygen and phosphorus elements, has relatively high adsorption capacity on various sulfonamide antibiotics, is relatively high in adsorption rate, and can be regenerated and recycled through regeneration treatment. The efficient adsorbent for the sulfonamide antibiotics, provided by the invention, is simple in preparation method and relatively low in cost, can be used for quickly and efficiently treating sewage containing the sulfonamide antibiotics, and has wide popularization and application prospects.
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Description

Technical Field

[0001] The invention belongs to the technical field of wastewater treatment, and specifically relates to a high-efficiency adsorbent for sulfonamide antibiotics and a preparation method and application thereof. Background Art

[0002] Sulfonamide antibiotics are a general term for aminobenzenesulfonamide and its various derivatives. They are synthetic antibiotics. Except for sulfonamide, which is alkaline, the rest are amphoteric substances. Their antibacterial activity mainly depends on the amino group (N 4 ) on R 2 R 1 Sulfonamide antibiotics are broad-spectrum antibiotics with excellent antibacterial activity against most Gram-positive and Gram-negative bacteria.

[0003] Sulfonamide antibiotics are widely used in human medical, livestock and poultry, and aquaculture to prevent and treat bacterial infections. In the medical industry, the demand and use of sulfonamide antibiotics are large, and wastewater containing sulfonamide antibiotics generated during the pharmaceutical production process is discharged into the environment in large quantities; in the livestock and poultry and aquaculture industries, about 85% of antibiotics cannot be absorbed and are excreted in the form of prototypes or metabolites with animal feces and urine, and still have biological activity, which can change the genetic characteristics of the microbial system and cause poisoning. In domestic sewage and surface waters around sewage treatment plants, the concentration level of sulfonamide antibiotics can reach the μg / L level. Sulfonamide antibiotics can be enriched in the environment, causing long-term damage to the ecology. Therefore, effective methods must be used to remove sulfonamide antibiotics from water to ensure people's healthy lives.

[0004] There are many methods for treating sulfonamide antibiotics pollutants, such as adsorption, electrochemical method, MBR method, upflow anaerobic sludge blanket method, etc. Among them, adsorption is one of the most efficient and simple methods for removing sulfonamide antibiotics from wastewater. However, the adsorption efficiency of common porous materials for sulfonamide antibiotics is not ideal. Therefore, it is particularly important to seek efficient adsorbents.

[0005] The main reasons for the unsatisfactory adsorption efficiency of porous materials for sulfonamide antibiotics are as follows: First, the surface chemistry regulation of traditional adsorbents is relatively difficult, and the specific surface area is easily affected after modification, resulting in low adsorption capacity; for example: Patent document with application number 201910783672.7 discloses a preparation method of an ionic liquid functionalized metal organic framework-molecular imprinting composite material, the theoretical maximum adsorption capacity of the adsorbent for sulfamethoxazole is 60.88umol / g, the theoretical maximum adsorption capacity for sulfamethoxazole is 37.20umol / g, and the theoretical maximum adsorption capacity for sulfadiazine is close to 37.77umol / g. The adsorption reaches equilibrium in about 3h, and the adsorption capacity is small; second, most adsorbents are limited by pore structure, resulting in a slow adsorption rate of sulfonamide antibiotics by the adsorbent; for example: Patent document with application number 201810383270.3 discloses a method for adding graphene oxide as a raw material to a thiourea solution , after sufficient mixing to remove thiourea impurities, a new type of reductive graphene material rich in nitrogen and sulfur elements was prepared. The maximum adsorption capacity of the adsorbent for sulfamethoxazole (SMZ) is 100.26 mg / g, the maximum adsorption capacity for sulfapyridine (SFD) is close to 80 mg / g, and the maximum adsorption capacity for sulfadiazine (SFZ) is close to 98 mg / g, but it takes about 50 hours for the adsorption to reach equilibrium. Not only is the adsorption amount small, but the time to reach adsorption equilibrium is long; third, the adsorbent is complicated to make, and the cost is relatively high; for example: The patent document with application number 202110025476.0 discloses a preparation method and application of an antibiotic rapid adsorbent, which prepares an adsorbent for rapid adsorption of antibiotics. The time for the adsorbent to reach adsorption equilibrium is 25 minutes, but it is necessary to first prepare an intermediate by electrospinning and then calcine at high temperature. The preparation process is complicated, and it is uncertain whether it has regeneration performance, which limits the large-scale application of the material. Patent document with application number 202311661881.7 discloses a cubic bifunctional adsorption material, a preparation method and application thereof. The adsorption equilibrium is reached in 5 hours, and the removal efficiency of sulfonamide antibiotics reaches 90%. However, the zeolite imidazole skeleton needs to be heated to above 800°C under inert gas for calcination to obtain the cubic bifunctional adsorption material. The basic raw materials are expensive and the cost is high, which greatly limits the application of this material.

[0006] Based on this, it is a technical problem that urgently needs to be solved to provide a sulfonamide antibiotic adsorbent and a preparation method thereof with a simple preparation method, mild reaction conditions, large specific surface area, rich pores, and high adsorption rate, so as to achieve rapid and efficient treatment of wastewater containing sulfonamide antibiotics. Summary of the invention

[0007] One of the purposes of the present invention is to provide a method for preparing a high-efficiency adsorbent for sulfonamide antibiotics, which has a simple preparation method, mild reaction conditions, large specific surface area, rich pores and high adsorption rate.

[0008] The second object of the present invention is to provide a high-efficiency adsorbent for sulfonamide antibiotics with a simple preparation method, mild reaction conditions, large specific surface area, rich pores and high adsorption rate.

[0009] The third object of the present invention is to provide an application of a highly efficient adsorbent for sulfonamide antibiotics.

[0010] The technical solution adopted by the present invention to achieve one of the purposes is: to provide a method for preparing a high-efficiency adsorbent for sulfonamide antibiotics, comprising the following steps: adding tetrabenzyl phosphate, a cross-linking agent, an auxiliary agent and a catalyst into a solvent in a molar ratio of 1:(8-10):(1-3):(4-6), carrying out a Friedel-Crafts alkylation reaction at 60-100° C. for a reaction time of 12-36 hours to obtain a product; and purifying the product to obtain a porous adsorbent.

[0011] In the preparation method of the adsorbent provided by the present invention, tetrabenzyl phosphate is used as a monomer. The material structure has four benzyl rings, which can significantly increase the specific surface area of ​​the synthetic adsorbent. In addition, tetrabenzyl phosphate also contains a large amount of phosphorus and oxygen. These heteroelements can form hydrogen bonds with sulfonamide antibiotics to enhance the adsorption effect.

[0012] Furthermore, the cross-linking agent is selected from a combination of one or more of dimethoxymethane, trimethyl orthoformate, and 1,4-benzenedimethanol.

[0013] Furthermore, the catalyst is ferric chloride and / or aluminum chloride.

[0014] Furthermore, the solvent is selected from a combination of one or more selected from chloroform, dichloromethane, and dichloroethane.

[0015] Further, the concentration of tetrabenzyl phosphate in the solvent is 0.02-0.05 g / mL. Preferably, the concentration of tetrabenzyl phosphate in the solvent is 0.03-0.04 g / mL.

[0016] Furthermore, the auxiliary agent is selected from a combination of one or more of benzene, biphenyl, 1,4-terphenyl, tetracene, and pyrene. In the present invention, the addition of auxiliary agents can further increase the specific surface area of ​​the product. It has been found that when no auxiliary agent is added, the adsorbent product obtained has the highest oxygen and phosphorus content, but the specific surface area is small; and as the amount of auxiliary agent increases, the specific surface area also increases. Taking into account the product area and oxygen and phosphorus content, the molar ratio of tetrabenzyl phosphate to the auxiliary agent is limited to 1: (1-3). At this time, the prepared adsorbent not only has a higher specific surface area, but also has a higher content of heteroelements, so that it can exert a better adsorption effect on sulfonamide antibiotics.

[0017] Preferably, the temperature of the Friedel-Crafts alkylation reaction is 70-90° C. and the time is 18-24 h.

[0018] Furthermore, the purification process includes washing, Soxhlet extraction and drying in sequence.

[0019] Preferably, the washing solvent is selected from a combination of one or more of water, methanol, ethanol, acetone and ether; more preferably, the washing solvent is methanol.

[0020] Preferably, in the Soxhlet extraction, the extraction solvent is selected from a combination of one or more of methanol, ethanol, acetone and ether; more preferably, methanol is used as the extraction solvent.

[0021] Preferably, the drying process is carried out at a temperature of 60-90°C and for a time of 15-24 hours.

[0022] The technical solution adopted by the present invention to achieve the second purpose is: to provide a high-efficiency adsorbent for sulfonamide antibiotics, which is prepared by the preparation method according to one of the purposes of the present invention.

[0023] Furthermore, the sulfonamide antibiotics efficient adsorbent comprises a plurality of open and ordered 3D channels formed by the accumulation of nanoparticles. The channels are composed of a main pore structure with a pore size of 0.5-8 nm and a small amount of pore structures with a pore size of 5-30 nm. This 3D nanopore structure with multiple pore sizes enables the adsorbent prepared by the present invention to have a larger specific surface area and higher adsorption activity.

[0024] The technical solution adopted by the present invention to achieve the third purpose is: to provide an application of the high-efficiency adsorbent for sulfonamide antibiotics according to the second purpose of the present invention. The application includes: applying the high-efficiency adsorbent for sulfonamide antibiotics to the adsorption treatment of sulfonamide antibiotics.

[0025] Furthermore, the sulfonamide antibiotics include a combination of one or more of sulfamethoxazole, sulfapyridine and sulfadiazine.

[0026] Preferably, the adsorption treatment method comprises: dispersing the adsorbent in a solution containing sulfonamide antibiotics at room temperature, mixing the solution and allowing it to stand for adsorption.

[0027] Preferably, in the solution containing sulfonamide antibiotics, the concentration of sulfonamide antibiotics is 300-500 mg / L, the amount of adsorbent added to the solution containing sulfonamide antibiotics is 0.1-2 g / L, and the static adsorption time is 0.1-1 h.

[0028] Furthermore, the application also includes regenerating the used sulfonamide antibiotics high-efficiency adsorbent; the regenerating treatment includes: washing the used sulfonamide antibiotics high-efficiency adsorbent several times with a regenerating solvent, and then drying it.

[0029] Furthermore, the regeneration solvent includes a combination of one or more of ethyl acetate, deionized water, methanol, and NaOH solution.

[0030] Preferably, the regeneration solvent is selected from ethyl acetate or a 0.01 mol / L NaOH aqueous solution. Ethyl acetate can form hydrogen bonds with sulfonamide in the adsorbent and remove it, and then directly filter and dry it to complete the regeneration process; when 0.01 mol / L NaOH is used as the regeneration solvent, based on the principle that sulfonamide antibiotics have good solubility in alkaline solutions, the sulfonamide antibiotics in the adsorbent are removed, and then the adsorbent is fully washed with water and dried to complete the regeneration process.

[0031] Preferably, the washing temperature is 40-80°C, the drying temperature is 40-80°C, and the drying time is 10-24h.

[0032] Furthermore, after five cycles of regeneration treatment, the high-efficiency adsorbent for sulfonamide antibiotics prepared by the present invention maintains an adsorption amount of sulfonamide antibiotics at 92.01%-94.51% of the original adsorption amount, showing a good regeneration and recycling effect.

[0033] Compared with the prior art, the present invention has the following beneficial effects: (1) The preparation method of the high-efficiency adsorbent for sulfonamide antibiotics provided by the present invention adopts a one-pot method, uses tetrabenzyl phosphate compound as the main raw material, and performs Friedel-Crafts alkylation reaction to obtain a high-efficiency adsorbent containing phosphorus and oxygen. The preparation method is simple, the reaction conditions are mild, it is environmentally friendly, and it has good applicability.

[0034] (2) The high-efficiency adsorbent for sulfonamide antibiotics prepared by the present invention has a high specific surface area and contains a multi-level pore structure. The adsorbent has a high content of heteroatom phosphorus and oxygen, can exhibit excellent adsorption capacity and adsorption rate for a variety of sulfonamide antibiotics, and can achieve good regeneration and recycling effects, and has important application and promotion value. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 This is a nitrogen adsorption-desorption curve diagram of the adsorbent prepared in Example 1 of the present invention; Figure 2 This is a pore size distribution diagram of the adsorbent prepared in Example 1 of the present invention; Figure 3This is a scanning electron microscope image of the adsorbent prepared in Example 1 of the present invention; Figure 4 The adsorption kinetic curve of desulfurized methoxazole prepared in Example 1 of the present invention; Figure 5 The 303K isothermal adsorption curves of sulfamethoxazole, sulfadiazine and sulfapyridine of the adsorbent prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0036] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. 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 making creative work are within the scope of protection of the present invention.

[0037] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments may be combined with each other.

[0038] The present invention will be further described below in conjunction with specific embodiments, but the present invention is not limited thereto.

[0039] The main parameters and variables involved in the embodiments and comparative examples of the present invention are shown in Table 1 below: Table 1

[0040] Example 1 A high-efficiency adsorbent for sulfonamide antibiotics, the preparation method of which comprises the following steps: Step 1: Add 5.3847 g of tetrabenzyl phosphate to a single-necked flask, then add 300 mL of 1,2-dichloroethane, and dissolve the tetrabenzyl phosphate by ultrasonication to obtain a solution; Step 2: Add 7.01 g of dimethoxymethane as a crosslinking agent, 8.2 g of anhydrous ferric chloride as a catalyst, and 1.01 g of benzene as an auxiliary agent to the solution obtained in step 1, and then place in an oil bath at 80° C. and react for 24 hours under magnetic stirring to obtain a crude polymer product; Step 3: The crude polymer product obtained in step 2 is washed three times with 200 mL of methanol to remove a large amount of anhydrous ferric chloride, and then extracted with a methanol Soxhlet extractor until the extract is colorless, and then rotary evaporated at 60° C. for 12 hours to obtain a highly efficient adsorbent for sulfonamide antibiotics.

[0041] Figure 1 The nitrogen adsorption-desorption curve of the adsorbent prepared in Example 1 is Figure 1 It can be seen that the adsorbent prepared in Example 1 has a relatively high specific surface area of ​​1047 m 2 / g.

[0042] Figure 2 The pore distribution diagram of the adsorbent prepared in Example 1 is shown in FIG. Figure 2 It can be seen that the porous adsorbent prepared in Example 1 has a good pore structure, the main pores of which are nanopore structures with a pore size of 0.5-8nm, and it also contains a small amount of pore structures with a pore size of 5nm-30nm. The nanopore structures with various pore sizes make the porous adsorbent have a larger specific surface area and higher adsorption activity.

[0043] Figure 3 This is a scanning electron microscope image of the adsorbent prepared in Example 1. Figure 3 It can be seen that the adsorbent prepared in Example 1 is composed of nano-scale particles stacked to form open and ordered 3D channels.

[0044] Figure 4 The adsorption kinetic curve of desulfurized methoxazole prepared in Example 1 is as follows: Figure 4 It can be seen that the porous adsorbent can reach adsorption equilibrium for sulfamethoxazole in 30 minutes, and the adsorption rate is relatively fast.

[0045] Figure 5 The adsorption isotherm curves of sulfamethoxazole, sulfapyridine and sulfadiazine prepared in Example 1 are as follows: Figure 5 It can be seen that the maximum adsorption capacity of the porous adsorbent for sulfamethoxazole is 328 mg / g; the maximum adsorption capacity for sulfapyridine is 238 mg / g; and the maximum adsorption capacity for sulfadiazine is 282 mg / g.

[0046] Example 2 A high-efficiency adsorbent for sulfonamide antibiotics, the preparation method of which comprises the following steps: Step 1: Add 5.3847 g of tetrabenzyl phosphate to a single-necked flask, then add 300 mL of 1,2-dichloroethane, and dissolve the tetrabenzyl phosphate by ultrasonication to obtain a solution; Step 2: Add 7.01 g of dimethoxymethane as a crosslinking agent, 8.2 g of anhydrous ferric chloride as a catalyst, and 2.02 g of benzene as an auxiliary agent to the solution obtained in step 1, and then place in an oil bath at 80° C. and react for 24 hours under magnetic stirring to obtain a crude polymer product; Step 3: The crude polymer product obtained in step 2 is washed three times with 200 mL of methanol to remove a large amount of anhydrous ferric chloride, and then extracted with a methanol Soxhlet extractor until the extract is colorless, and then rotary evaporated at 60° C. for 12 hours to obtain a highly efficient adsorbent for sulfonamide antibiotics.

[0047] Example 3 A high-efficiency adsorbent for sulfonamide antibiotics, the preparation method of which comprises the following steps: Step 1: Add 5.3847 g of tetrabenzyl phosphate to a single-necked flask, then add 500 mL of 1,2-dichloroethane, and dissolve the tetrabenzyl phosphate by ultrasonication to obtain a solution; Step 2: Add 6.08 g of dimethoxymethane as a crosslinking agent, 6.5 g of anhydrous ferric chloride as a catalyst, and 0.78 g of benzene as an auxiliary agent to the solution obtained in step 1, and then place in an oil bath at 80° C. and react for 24 hours under magnetic stirring to obtain a crude polymer product; Step 3: The crude polymer product obtained in step 2 is washed three times with 200 mL of methanol to remove a large amount of anhydrous ferric chloride, and then extracted with a methanol Soxhlet extractor until the extract is colorless, and then rotary evaporated at 60° C. for 12 hours to obtain a highly efficient adsorbent for sulfonamide antibiotics.

[0048] Example 4 A high-efficiency adsorbent for sulfonamide antibiotics, the preparation method of which comprises the following steps: Step 1: Add 5.3847 g of tetrabenzyl phosphate to a single-necked flask, then add 200 mL of 1,2-dichloroethane, and dissolve the tetrabenzyl phosphate by ultrasonication to obtain a solution; Step 2: Add 7.61 g of dimethoxymethane as a crosslinking agent, 9.7 g of anhydrous ferric chloride as a catalyst, and 2.34 g of benzene as an auxiliary agent to the solution obtained in step 1, and then place in an oil bath at 80° C. and react for 24 hours under magnetic stirring to obtain a crude polymer product; Step 3: The crude polymer product obtained in step 2 is washed three times with 200 mL of methanol to remove a large amount of anhydrous ferric chloride, and then extracted with a methanol Soxhlet extractor until the extract is colorless, and then rotary evaporated at 60° C. for 12 hours to obtain a highly efficient adsorbent for sulfonamide antibiotics.

[0049] Comparative Example This comparative example provides a sulfonamide antibiotic adsorbent, which is mainly different from Example 1 in that 1.01 g of benzene is not added as an auxiliary agent in step 2, and its preparation method comprises the following steps: Step 1: Add 5.3847 g of tetrabenzyl phosphate to a single-necked flask, then add 300 mL of 1,2-dichloroethane, and dissolve the tetrabenzyl phosphate by ultrasonication to obtain a solution; Step 2: Add 7.01 g of dimethoxymethane as a crosslinking agent and 8.2 g of anhydrous ferric chloride as a catalyst to the solution obtained in step 1, then place in an oil bath at 80° C. and react for 24 hours under magnetic stirring to obtain a crude polymer product; Step 3: The crude polymer product obtained in step 2 is washed three times with 200 mL of methanol to remove a large amount of anhydrous ferric chloride, and then extracted with a methanol Soxhlet extractor until the extract is colorless, and then rotary evaporated at 60° C. for 12 h to obtain a sulfonamide antibiotic adsorbent.

[0050] Application performance testing 1. Adsorption capacity test The adsorbents prepared in Examples 1-4 and the comparative example were added to sewage containing different types of sulfonamide antibiotics at a mass ratio of 0.001:1, and the concentration of sulfonamide antibiotics in the sewage was 350 mg / L. The adsorption temperature was controlled at 30°C and the adsorption time was 30 min. The test results of the adsorption capacity of the adsorbents prepared in Examples 1-4 and the comparative example for sulfonamide antibiotics are shown in Table 2 below.

[0051] Table 2

[0052] As can be seen from the above table, The adsorbents prepared in Examples 1-4 of the present invention have a high specific surface area, a multi-level pore structure, and abundant oxygen and phosphorus elements. Based on the above advantages, the adsorbent has a high adsorption capacity for a variety of sulfonamide antibiotics and a fast adsorption rate, and can reach an adsorption amount of 219-328 mg / g within 30 minutes.

[0053] Further, by comparing the test results of Example 1 with the comparative example, it can be seen that the comparative example does not contain auxiliary benzene in the raw material, although the oxygen and phosphorus content in the prepared adsorbent is higher, the specific surface area is small, and the adsorption amount is limited; Example 1 adds a certain amount of auxiliary benzene on the basis of the comparative example, and the adsorption amount of sulfonamide antibiotics by the prepared adsorbent is significantly improved, which shows that the addition of auxiliary benzene increases the surface area of ​​the adsorbent, and thus has a positive effect on the adsorption capacity. Example 2 increases the content of auxiliary benzene on the basis of Example 1, and the adsorption amount is reduced compared with Example 1, which shows that the addition of auxiliary benzene needs to be controlled within a reasonable range. Although excessive benzene can further increase the specific surface area of ​​the product, it will cause the oxygen and phosphorus content in the product to decrease, thereby affecting the adsorption effect.

[0054] (II) Adsorption capacity test after regeneration treatment The highly efficient porous adsorbent of Example 1 that adsorbs organic matter containing sulfonamide antibiotics in the application performance test is recovered and subjected to a cyclic regeneration application test. Specifically, the following steps are included: at 60°C, 0.01 g of the adsorbent obtained in Example 1 after adsorbing sulfamethoxazole, sulfapyridine, and sulfadiazine is washed with 100 mL of ethyl acetate respectively; after washing three times, it is dried at 60°C for 12 hours to obtain a regenerated adsorbent; the adsorption performance of the regenerated adsorbent is tested and the substrate concentration in the residual liquid is measured, and the results are shown in Table 3 below: Table 3

[0055] As can be seen from the above table, The sulfonamide antibiotics high-efficiency adsorbent prepared by the present invention still maintains a relatively high adsorption amount after multiple regeneration treatments. For a sulfamethoxazole aqueous solution system, the adsorption amount after five regeneration treatments is 94.51% of the original adsorption amount; for a sulfapyridine aqueous solution system, the adsorption amount after five regeneration treatments is 92.01% of the original adsorption amount; for a sulfadiazine aqueous solution system, the adsorption amount after five regeneration treatments is 93.97% of the original adsorption amount, showing a good regeneration and recycling effect, and having important application and promotion value.

[0056] The above are only preferred embodiments of the present invention, and are not intended to limit the implementation methods and protection scope of the present invention. Those skilled in the art should be aware that all solutions obtained by equivalent substitutions and obvious changes made using the contents of the specification of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a highly efficient adsorbent for sulfonamide antibiotics, characterized in that: The following steps are involved: Tetrabenzyl phosphate, a crosslinking agent, an auxiliary agent and a catalyst are added to a solvent in a molar ratio of 1:(8-10):(1-3):(4-6), and a Friedel-Crafts alkylation reaction is carried out at 60-100° C. for 12-36 hours to obtain a product; the product is purified to obtain a porous adsorbent.

2. The preparation method according to claim 1, characterized in that: The cross-linking agent is selected from the group consisting of one or more combinations of dimethoxymethane, trimethyl orthoformate, and 1,4-benzenedimethanol.

3. The preparation method according to claim 1, characterized in that: The catalyst is ferric chloride and / or aluminum chloride.

4. The preparation method according to claim 1, characterized in that: The solvent is selected from a combination of one or more selected from chloroform, dichloromethane, and dichloroethane.

5. The preparation method according to claim 1, characterized in that: The auxiliary agent is selected from one or more combinations of benzene, biphenyl, 1,4-terphenyl, tetracene and pyrene.

6. The preparation method according to claim 1, characterized in that: The concentration of tetrabenzyl phosphate in the solvent is 0.02-0.05 g / mL.

7. The preparation method according to claim 1, characterized in that: The purification process includes washing, Soxhlet extraction and drying in sequence.

8. A highly efficient adsorbent for sulfonamide antibiotics, prepared by the preparation method according to any one of claims 1 to 7, characterized in that: The sulfonamide antibiotics high-efficiency adsorbent comprises a plurality of open and ordered 3D channels formed by the accumulation of nanoparticles. The 3D channels consist of a main pore structure with a pore size of 0.5-8 nm and a small amount of pore structures with a pore size of 5-30 nm.

9. An application of the high-efficiency adsorbent for sulfonamide antibiotics according to claim 8, characterized in that: The high-efficiency adsorbent for sulfonamide antibiotics is applied to the adsorption treatment of sulfonamide antibiotics; the sulfonamide antibiotics include a combination of one or more of sulfamethoxazole, sulfapyridine and sulfadiazine.

10. The use according to claim 9, characterized in that: The application also includes regenerating the used high-efficiency adsorbent for sulfonamide antibiotics; the regenerating treatment includes: washing the used high-efficiency adsorbent for sulfonamide antibiotics several times with a regenerating solvent and drying it; the regenerating solvent includes a combination of one or more of ethyl acetate, deionized water, methanol, and NaOH solution.

Citation Information

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